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Sample records for simultaneous sensitive determination

  1. Single-acquisition method for simultaneous determination of extrinsic gamma-camera sensitivity and spatial resolution

    Energy Technology Data Exchange (ETDEWEB)

    Santos, J.A.M. [Servico de Fisica Medica, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal)], E-mail: a.miranda@portugalmail.pt; Sarmento, S. [Servico de Fisica Medica, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Alves, P.; Torres, M.C. [Departamento de Fisica da Universidade do Porto, Rua do Campo Alegre 687, 4169-007 Porto (Portugal); Bastos, A.L. [Servico de Medicina Nuclear, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Ponte, F. [Servico de Fisica Medica, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal)

    2008-01-15

    A new method for measuring simultaneously both the extrinsic sensitivity and spatial resolution of a gamma-camera in a single planar acquisition was implemented. A dual-purpose phantom (SR phantom; sensitivity/resolution) was developed, tested and the results compared with other conventional methods used for separate determination of these two important image quality parameters. The SR phantom yielded reproducible and accurate results, allowing an immediate visual inspection of the spatial resolution as well as the quantitative determination of the contrast for six different spatial frequencies. It also proved to be useful in the estimation of the modulation transfer function (MTF) of the image formation collimator/detector system at six different frequencies and can be used to estimate the spatial resolution as function of the direction relative to the digital matrix of the detector.

  2. Single-acquisition method for simultaneous determination of extrinsic gamma-camera sensitivity and spatial resolution

    International Nuclear Information System (INIS)

    Santos, J.A.M.; Sarmento, S.; Alves, P.; Torres, M.C.; Bastos, A.L.; Ponte, F.

    2008-01-01

    A new method for measuring simultaneously both the extrinsic sensitivity and spatial resolution of a gamma-camera in a single planar acquisition was implemented. A dual-purpose phantom (SR phantom; sensitivity/resolution) was developed, tested and the results compared with other conventional methods used for separate determination of these two important image quality parameters. The SR phantom yielded reproducible and accurate results, allowing an immediate visual inspection of the spatial resolution as well as the quantitative determination of the contrast for six different spatial frequencies. It also proved to be useful in the estimation of the modulation transfer function (MTF) of the image formation collimator/detector system at six different frequencies and can be used to estimate the spatial resolution as function of the direction relative to the digital matrix of the detector

  3. Sensitive double-antibody method for simultaneous determination of insulin and growth hormone

    International Nuclear Information System (INIS)

    Koparanova, O.; Sotirov, G.; Tyrkolev, N.

    1982-01-01

    A method is described for simultaneous determination of insulin and growth hormone in one sample, using double-antibody technique. The method is characterized by appreciable sensitivity (2.5 μE/ml for insulin and a.2 ng/ml for growth hormone), exactness (variation quotient 6-16 per cent) and reproducibility (96.9-117 per cent). There was no statistically significant difference in the insulin and growth hormone values of the same sera, determined by the here suggested and the standard methods. The necessary test material for examination of either hormone is minimal (0.2 ml). One may thus extend the possibilities for radioimmunologic determination of insulin and growth hormone, when only minor amounts of serum or other biological fluid are available. The method is also less time consuming. Results are reported of statistical processing of an experimental model and different sera determined by the standard method and the one described by the authors. (author)

  4. Simultaneous Determination of Famotidine and Flurbiprofen by High ...

    African Journals Online (AJOL)

    Purpose: To develop a selective, sensitive and accurate simultaneous High Performance Liquid Chromatography (HPLC) method for the analysis of flurbiprofen and famotidine tablet dosage form and excipients. Methods: A simultaneous method for the determination of the two drugs was employed. The assay consisted of ...

  5. Simultaneous spectrophotometric determination of tungsten and molybdenum with dithiol

    International Nuclear Information System (INIS)

    Navale, A.S.

    1987-01-01

    Toluene-3,4-dithiol is a very sensitive reagent for the spectrophotometric determination of tungsten and molybdenum. Since the absorption spectra of the dithiol complexes of these two elements overlap, a separation of the two elements is carried out. This leads to time consuming extraction procedures. Measuring the absorption of the mixed complexes at two wavelengths and solving a set of simultaneous equations is also not favorable because a lot of time and effort is required for solving the simultaneous equations for each sample. A faster and simpler method is described here for the simultaneous determination of the two elements. The method is based on measurement of absorbance of the mixed complexes at three pre-selected wavelengths and simple calculations involving the absorbance differences. The criteria for selecting the three wavelengths and the theory are described. Application of the method for the determination of tungsten and molybdenum in ore samples is presented. The method is applicable to any similar system consisting of two interfering components. 4 figures, 2 tables, 6 refs. (author)

  6. SIMULTANEOUS SPECTROPHOTOMETRIC DETERMINATION OF MONTELUKAST SODIUM AND BAMBUTEROL HYDROCHLORIDE IN TABLETS

    OpenAIRE

    Patel Satish A; Patel Dhara J; Patel Natavarlal J.

    2011-01-01

    The present manuscript describe simple, sensitive, rapid, accurate, precise and economical first derivative spectrophotometric method for the simultaneous determination of montelukast sodium and bambuterol hydrochloride in combined tablet dosage form. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra was obtained in chloroform and the determinations were made at 241 nm (ZC...

  7. Highly sensitive and simultaneous electrochemical determination of 2-aminophenol and 4-aminophenol based on poly(l-arginine)-β-cyclodextrin/carbon nanotubes@graphene nanoribbons modified electrode.

    Science.gov (United States)

    Yi, Yinhui; Zhu, Gangbing; Wu, Xiangyang; Wang, Kun

    2016-03-15

    Owing to the similar characteristics and physiochemical property of 2-aminophenol (2-AP) and 4-aminophenol (4-AP), the highly sensitive simultaneous electrochemical determination of 2- and 4-AP is a great challenge. In this paper, by electropolymerizing β-cyclodextrin (β-CD) and l-arginine (l-Arg) on the surface of carbon nanotubes@graphene nanoribbons (CNTs@GNRs) core-shell heterostructure, a P-β-CD-l-Arg/CNTs@GNRs nanohybrid modified electrode was prepared successfully, and it could exhibit the synergetic effects of β-CD (high host-guest recognition and enrichment ability), l-Arg (excellent electrocatalytic activity) and CNTs@GNRs (prominent electrochemical properties and large surface area), the P-β-CD-l-Arg/CNTs@GNRs modified electrode was used in the electrochemical determination of 2- and 4-AP, the results demonstrated that the highly sensitive and simultaneous determination of 2- and 4-AP is successfully achieved and the modified electrode has a linear response range of 25.0-1300.0 nM for both 2- and 4-AP, and the detection limits of 2- and 4-AP obtained in this work are 6.2 and 3.5 nM, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Sensitive electrochemical sensors for simultaneous determination of ascorbic acid, dopamine, and uric acid based on Au@Pd-reduced graphene oxide nanocomposites

    Science.gov (United States)

    Jiang, Jingjing; Du, Xuezhong

    2014-09-01

    Sensitive electrochemical sensors were fabricated with reduced graphene oxide-supported Au@Pd (Au@Pd-RGO) nanocomposites by one-step synthesis for individual and simultaneous determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA) with low detection limits and wide concentration ranges. From the Au@Pd-RGO-modified electrodes, well-separated oxidation peaks and enhanced peak currents of AA, DA, and UA were observed owing to the superior conductivity of RGO and the excellent catalytic activity of Au@Pd nanoparticles. For individual detection, the linear responses of AA, DA, and UA were in the concentration ranges of 0.1-1000, 0.01-100, and 0.02-500 μM with detection limits of 0.02, 0.002, and 0.005 μM (S/N = 3), respectively. For simultaneous detection by synchronous change of the concentrations of AA, DA, and UA, the linear response ranges were 1-800, 0.1-100, and 0.1-350 μM with detection limits of 0.28, 0.024, and 0.02 μM (S/N = 3), respectively. The fabricated sensors were further applied to the detection of AA, DA, and UA in urine samples. The Au@Pd-RGO nanocomposites have promising applications in highly sensitive and selective electrochemical sensing.Sensitive electrochemical sensors were fabricated with reduced graphene oxide-supported Au@Pd (Au@Pd-RGO) nanocomposites by one-step synthesis for individual and simultaneous determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA) with low detection limits and wide concentration ranges. From the Au@Pd-RGO-modified electrodes, well-separated oxidation peaks and enhanced peak currents of AA, DA, and UA were observed owing to the superior conductivity of RGO and the excellent catalytic activity of Au@Pd nanoparticles. For individual detection, the linear responses of AA, DA, and UA were in the concentration ranges of 0.1-1000, 0.01-100, and 0.02-500 μM with detection limits of 0.02, 0.002, and 0.005 μM (S/N = 3), respectively. For simultaneous detection by synchronous change of the

  9. A sensitive liquid chromatography-mass spectrometry method for the simultaneous determination in plasma of pentacyclic triterpenes of Olea europaea L.

    Science.gov (United States)

    Giménez, Estela; Juan, M Emília; Calvo-Melià, Sara; Planas, Joana M

    2017-08-15

    Table olives are especially rich in pentacyclic triterpenic compounds, which exert several biological activities. A crucial step in order to know if these compounds could contribute to the beneficial and healthy properties of this food is their measurement in blood. Therefore, the present study describes a simple and accurate liquid-liquid extraction followed by LC-QqQ-MS analysis for the simultaneous determination of the main pentacyclic triterpenes from Olea europaea L. in rat plasma. The method was validated by the analysis of blank plasma samples spiked with pure compounds, obtaining a linear correlation, adequate sensitivity with a limit of quantification ranging from 1nM for maslinic acid to 10nM for uvaol. Precision and accuracy were lower than 10% in all cases and recoveries were between 95 and 104%. The oral administration of olives to rats and its determination in plasma verified that the established methodology is appropriate for bioavailability studies. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Simultaneous determination of paracetamol and penicillin V by square-wave voltammetry at a bare boron-doped diamond electrode

    International Nuclear Information System (INIS)

    Švorc, Ľubomír; Sochr, Jozef; Tomčík, Peter; Rievaj, Miroslav; Bustin, Dušan

    2012-01-01

    Highlights: ► Unmodified BDD electrode = sensitive electrochemical sensor for drugs determination. ► No special pretreatment of samples except simple dilution. ► Selective method, common compounds present in urine do not interfere in high excess. ► Simultaneous determination of PAR and PEN has yet not been published in literature. - Abstract: A simple, sensitive and selective square-wave voltammetry method for simultaneous determination of paracetamol and penicillin V on a bare (unmodified) boron-doped diamond electrode has been developed. The good potential separation of about 0.35 V between the oxidation peak potentials of both drugs present in mixture was found. It was found by cyclic voltammetry that paracetamol gave quasireversible wave and penicillin V provided irreversible oxidation peak. The effect of supporting electrolyte, pH and scan rate on voltammetric response of both drugs was studied to select the optimum experimental conditions. The optimal conditions for quantitative simultaneous determination were obtained in acetate buffer solution at pH 5.0. The oxidation peak of paracetamol and penicillin V showed a systematic increase in peak currents with increase of their concentration. The calibration curves for the simultaneous determination of paracetamol and penicillin V exhibited the good linear responses within the concentration range from 0.4 to 100 μM for both drugs. The detection limit was established to 0.21 and 0.32 μM for paracetamol and penicillin V, respectively. The method proved the good sensitivity, repeatability (RSD of 1.5 and 2.1% for mixture solution of 10 μM PCM and PEN) and selectivity when influence of interferents commonly existing in human urine was negligible. The practical analytical utility of proposed method was demonstrated by simultaneous determination of paracetamol and penicillin V in human urine samples, with results similar to those obtained using a high-performance liquid chromatography method as an

  11. Simultaneous Determination of Glass Transition Temperatures of Several Polymers.

    Science.gov (United States)

    He, Jiang; Liu, Wei; Huang, Yao-Xiong

    2016-01-01

    A simple and easy optical method is proposed for the determination of glass transition temperature (Tg) of polymers. Tg was determined using the technique of microsphere imaging to monitor the variation of the refractive index of polymer microsphere as a function of temperature. It was demonstrated that the method can eliminate most thermal lag and has sensitivity about six fold higher than the conventional method in Tg determination. So the determined Tg is more accurate and varies less with cooling/heating rate than that obtained by conventional methods. The most attractive character of the method is that it can simultaneously determine the Tg of several polymers in a single experiment, so it can greatly save experimental time and heating energy. The method is not only applicable for polymer microspheres, but also for the materials with arbitrary shapes. Therefore, it is expected to be broadly applied to different fundamental researches and practical applications of polymers.

  12. New highly sensitive method of simultaneous instrumental neutron activation determination of 12 microelements in vine

    International Nuclear Information System (INIS)

    Shoniya, N.I.

    1977-01-01

    The main principles and methods of simultaneous multi-element instrumental neutron activation determination of microelements in vine seeds are presented. The methods permit to carry out quantitative evaluation for every single corn of the seeds. It is shown that the method of instrumental neutron activation analysis with the utilization of a semiconductor spectrometer of high resolution and mini electronic computer permit to carry out serial determinations of 12 microelements in the individual corns of vine seeds of different sorts. This method will permit to determine the missing or excess content of this or that biologically important microelement in soils, plants, fruit and genetic material - seeds, and so to determine the optimum conditions of growing plants by applying microelement fertilizers as extra nutrient means

  13. Sensitive radioimmunoassay and enzyme-linked immunosorbent assay for the simultaneous determination of chloroquine and its metabolites in biological fluids

    International Nuclear Information System (INIS)

    Escande, C.; Chevalier, P.; Verdier, F.; Bourdon, R.

    1990-01-01

    Two new methods for the simultaneous determination of chloroquine and its two main metabolites (monodesethylchloroquine and bisdesethylchloroquine) in biological samples, radioimmunoassay (RIA) and enzyme-linked immunosorbent assay (ELISA), are described. Antiserum is produced in rabbits immunized with N-(2-carboxyethyl)desethylchloroquine:protein conjugate. Besides chloroquine, this antiserum recognizes with good affinity the two main metabolites, monodesethylchloroquine and bisdesethylchloroquine (70 and 40% of crossreaction, respectively). Amodiaquine cross reacts by 4.5%; cross reactions with monodesethylamodiaquine, bisdesethylamodiaquine, and other antimalarial drugs are less than 1%. No extraction step or sample preparation is required for either system. Sensitivity limits are, respectively, 0.70 nM (3 pg of chloroquine sulfate measured in 10 microL of plasma sample) for RIA, and 10 nM (22 pg of chloroquine sulfate measured in 5 microL of plasma sample) for ELISA. The interassay coefficients of variation are, respectively, less than 10 and less than 16% for RIA and ELISA in the range 14-410 nM (6-180 ng/mL). The results of both methods are well correlated (r = 0.97) and correlate with spectrophotometry (r = 0.98) and HPLC results (r = 0.93). Because of their high sensitivity, both methods can be used in the case of chloroquine poisoning and in the control of malaria prophylaxis and treatment

  14. Simultaneous Determination of Ciprofloxacin and Tinidazole in ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, sensitive and specific liquid chromatographic method with PDA detection for the simultaneous estimation of ciprofloxacin and tinidazole in tablet dosage form. Methods: Separation was achieved with an Agilent XDB C18, 250 × 4.60 mm 5 μ column, low pressure gradient mode with a ambient ...

  15. Liquid-phase exfoliated graphene as highly-sensitive sensor for simultaneous determination of endocrine disruptors: Diethylstilbestrol and estradiol

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Lintong; Cheng, Qin [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Chen, Danchao; Ma, Ming [Ningbo Entry-exit Inspection and Quarantine Bureau of China, Ningbo 315012 (China); Wu, Kangbing, E-mail: kbwu@hust.edu.cn [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2015-02-11

    Graphical abstract: - Highlights: • A novel electrochemical sensor was developed for diethylstilbestrol and estradiol. • Graphene prepared by solvent exfoliation greatly enhances the detection sensitivity. • The newly-developed method has promising application and the accuracy is good. - Abstract: It is quite important to develop convenient and rapid analytical methods for trace levels of endocrine disruptors because they heavily affect health and reproduction of humans and animals. Herein, graphene was easily prepared via one-step exfoliation using N-methyl-2-pyrrolidone as solvent, and then used to construct an electrochemical sensor for highly-sensitive detection of diethylstilbestrol (DES) and estradiol (E2). On the surface of prepared graphene film, two independent and greatly-increased oxidation waves were observed at 0.28 V and 0.49 V for DES and E2. The remarkable signal enlargements indicated that the detection sensitivity was improved significantly. The influences of pH value, amount of graphene and accumulation time on the oxidation signals of DES and E2 were discussed. As a result, a highly-sensitive and rapid electrochemical method was newly developed for simultaneous detection of DES and E2. The values of detection limit were evaluated to be 10.87 nM and 4.9 nM for DES and E2. Additionally, this new method was successfully used in lake water samples and the accuracy was satisfactory.

  16. Highly sensitive simultaneous electrochemical determination of trace amounts of Pb(II) and Cd(II) using a carbon paste electrode modified with multi-walled carbon nanotubes and a newly synthesized Schiff base

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Ghaedi, Hamed; Madrakian, Tayyebeh; Rezaeivala, Majid

    2013-01-01

    Highlights: ► A new chemically modified carbon paste electrode was constructed and used. ► A new Schiff base and multi-walled carbon nanotube was used as modifiers. ► The electrochemical properties of the modified electrode were studied. ► The electrode was used to the simultaneous determination of Pb 2+ and Cd 2+ . -- Abstract: A new chemically modified electrode was constructed for rapid, simple, accurate, selective and highly sensitive simultaneous determination of lead and cadmium using square wave anodic stripping voltammetry (SWASV). The electrode was prepared by incorporation of new synthesized Schiff base and multi-walled carbon nanotubes (MWCNT) in carbon paste electrode. The limit of detection was found to be 0.25 ng mL −1 and 0.74 ng mL −1 for Pb 2+ and Cd 2+ , respectively. The stability constants of the complexes of the ligand with several metal cations in ethanol medium were determined. The effects of different cations and anions on the simultaneous determination of metal ions were studied and it was found that the electrode is highly selective. The proposed chemically modified electrode was used for the determination of lead and cadmium in several foodstuffs and water samples

  17. Simultaneous determination of four food allergens using compact disc immunoassaying technology.

    Science.gov (United States)

    Badran, Ahmed Ali; Morais, Sergi; Maquieira, Ángel

    2017-03-01

    A multiplex competitive microimmunoassay for the simultaneous determination of gliadin, casein, β-lactoglobulin, and ovalbumin is presented. The assay in microarray format is performed on a DVD where the allergens are physisorbed on the polycarbonate surface of the disc. The immunointeraction is detected using a mixture of specific gold-labeled antibodies and the signal amplified with the silver enhancement method. The optical density of the precipitate, read by a DVD drive, is related to the concentration of the four allergens in sample. An optimized protocol for the simultaneous extraction of the allergen proteins from food samples is also addressed. The suitability of the method is demonstrated for the simultaneous quantitative extraction and determination of the targeted allergens in spiked baby foods, juices, and beers. The sensitivity (EC50) of the multiplexed assay was 0.04, 0.40, 0.08, and 0.16 mg L -1 for gliadin, casein, β-lactoglobulin, and ovalbumin, respectively, and the recovery results from the analysis of food samples ranged from 72 to 117%. A portable, easy-to-use, array-based bioanalytical method is developed for quantification of food allergens with a limit of detection below the accepted levels of the international legislations, which allows promotion of food safety and quality. Graphical abstract GLI Gliadin, CAS Casein, β-LAC β-lactoglobulin, OVA Ovalbumin.

  18. Simultaneous determination of naphthol isomers at poly(3-methylthiophene)-nano-Au modified electrode with the enhancement of surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Li, Linlin [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Shandong Institute for Product Quality Inspection, Jinan 250100 (China); Liu, Enli; Wang, Xiaolin; Chen, Jia [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Zhang, Xiaoli, E-mail: zhangxl@sdu.edu.cn [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2015-08-01

    A polymer film incorporated gold nanoparticle modified electrode was fabricated. The fabricated process involved eletrodeposition of gold nanoparticles and electropolymerization of the 3-methylthiophene (abbreviated 3MT) onto the glassy carbon electrode (GCE). The resulting electrode (P3MT-nano-Au/GCE) was characterized by scanning electron microscopy (SEM), and a simultaneous determination of naphthol isomers at P3MT-nano-Au/GCE was studied using semi-derivative voltammetry. Because of the synergistic effect of gold nanoparticles and poly(3MT), the sensitivity and distinguishability in the simultaneous determination of naphthol isomers were greatly increased. Besides, a further increase in the detecting sensitivity of naphthol isomers could be obtained in the presence of surfactant, cetyl trimethyl ammonium bromide (CTAB). Also, the role of different kinds of surfactants was texted and the action mechanism was discussed in detail. Under the optimal conditions, the linear calibration ranges of the determination of naphthols were 7.0 × 10{sup −7} to 1.5 × 10{sup −4} mol/L for 1-naphthol and 1.0 × 10{sup −6} to 1.5 × 10{sup −4} mol/L for 2-naphthol with detection limits of 1.0 × 10{sup −7} and 3.0 × 10{sup −7} mol/L (S/N = 3), respectively. - Highlights: • Nano-Au-polymer film was fabricated by eletrodeposition and electropolymerization. • Naphthol isomers were detected simultaneously. • Surfactant improved the sensitivity and selectivity.

  19. Validated spectrophotometric methods for simultaneous determination of troxerutin and carbazochrome in dosage form

    Science.gov (United States)

    Khattab, Fatma I.; Ramadan, Nesrin K.; Hegazy, Maha A.; Al-Ghobashy, Medhat A.; Ghoniem, Nermine S.

    2015-03-01

    Four simple, accurate, sensitive and precise spectrophotometric methods were developed and validated for simultaneous determination of Troxerutin (TXN) and Carbazochrome (CZM) in their bulk powders, laboratory prepared mixtures and pharmaceutical dosage forms. Method A is first derivative spectrophotometry (D1) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD1) where the peak amplitude at 248 for TXN and 439 nm for CZM were used for their determination. Method C is ratio subtraction (RS); in which TXN was determined at its λmax (352 nm) in the presence of CZM which was determined by D1 at 483.5 nm. While, method D is mean centering of the ratio spectra (MCR) in which the mean centered values at 300 nm and 340.0 nm were used for the two drugs in a respective order. The two compounds were simultaneously determined in the concentration ranges of 5.00-50.00 μg mL-1 and 0.5-10.0 μg mL-1 for TXN and CZM, respectively. The methods were validated according to the ICH guidelines and the results were statistically compared to the manufacturer's method.

  20. Simultaneous determination of actinides by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Cohen, V.H.

    1990-01-01

    The x-ray spectrometric simultaneous determination of uranium and plutonium in simulated Purex Process solutions is described. The method is accomplished by intensity measurements of the L α sub(1) lines. The thin film technique for sample preparation and thorium as an internal standard had been used. An evaporation technique had been also tested for low concentration uranium solutions. In the measurement range 0,05 - 130 U g/L, 0,5 - 20 Pu g/L linear calibration curves were effected. The standard deviation in the concentration range 10 to 130 g/L was 3,5%, 4% in the 1 to 10 g/L and 13% in 0,05 to 1 g/L for uranium determination and 4% for plutonium determination in the range of 1 to 20 g/L. The sensitivity of the method was about 3,62 μg to U and 3,95 μg to Pu. Uranium and plutonium do not reciprocally interfere with one another until U/Pu ≅ 90 m/m. The fission product as interfering elements were also verified. Finally, uranium and plutonium were determined in simulated Purex Process solutions within the requested accuracy for control method. (author)

  1. Fast determination of strontium-89 and strontium-90 by simultaneous Cerencov- and Proportional-Counting; Schnelle Bestimmung von Strontium-89 und Strontium-90 mittels simultaner Cerenkov- und Proportionalzaehlrohrmessung

    Energy Technology Data Exchange (ETDEWEB)

    Laerbusch, Karin; Wiezorek, Claus [Chemisches und Veterinaeruntersuchungsamt MEL, Muenster (Germany)

    2014-01-20

    The presented method for simultaneous determination of Sr 89 and Sr 90 combines the techniques of Cerencov- and Proportional-Counting. Due to the low limit of detection of the latter technique, the method is very sensitive for the total radiostrontium. The distribution among two measurement devices offers the advantage of time saving.

  2. Electrodeposited nitrogen-doped graphene/carbon nanotubes nanocomposite as enhancer for simultaneous and sensitive voltammetric determination of caffeine and vanillin

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Lin; Ding, Yaping, E-mail: wdingyp@sina.com; Jiang, Feng; Li, Li; Mo, Fan

    2014-06-23

    Graphical abstract: A nanocomposite of nitrogen-doped graphene (NGR) and nitrogen-doped carbon nanotubes (NCNTs) was first modified onto an electrode through electrodeposition method and employed to sensitively detect caffeine and vanillin simultaneously for the first time. - Highlights: • The first electrochemical sensor for caffeine (CAF) and vanillin (VAN). • NGR–NCNTs was modified through electrodeposition for the first time. • The sensor was qualified for real sample determination with satisfactory results. - Abstract: A nitrogen-doped graphene/carbon nanotubes (NGR–NCNTs) nanocomposite was employed into the study of the electrochemical sensor via electrodeposition for the first time. The morphology and structure of NGR–NCNTs nanocomposite were investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. Meanwhile, the electrochemical performance of the glassy carbon electrode (GCE) modified with electrodeposited NGR–NCNTs (ENGR–NCNTs/GCE) towards caffeine (CAF) and vanillin (VAN) determination was demonstrated by cyclic voltammetry (CV) and square wave voltammetry (SWV). Under optimal condition, ENGR–NCNTs/GCE exhibited a wide linearity of 0.06–50 μM for CAF and 0.01–10 μM for VAN with detection limits of 0.02 μM and 3.3 × 10{sup −3} μM, respectively. Furthermore, the application of the proposed sensor in food products was proven to be practical and reliable. The desirable results show that the ENGR–NCNTs nanocomposite has promising potential in electrocatalytic biosensor application.

  3. Electrodeposited nitrogen-doped graphene/carbon nanotubes nanocomposite as enhancer for simultaneous and sensitive voltammetric determination of caffeine and vanillin

    International Nuclear Information System (INIS)

    Jiang, Lin; Ding, Yaping; Jiang, Feng; Li, Li; Mo, Fan

    2014-01-01

    Graphical abstract: A nanocomposite of nitrogen-doped graphene (NGR) and nitrogen-doped carbon nanotubes (NCNTs) was first modified onto an electrode through electrodeposition method and employed to sensitively detect caffeine and vanillin simultaneously for the first time. - Highlights: • The first electrochemical sensor for caffeine (CAF) and vanillin (VAN). • NGR–NCNTs was modified through electrodeposition for the first time. • The sensor was qualified for real sample determination with satisfactory results. - Abstract: A nitrogen-doped graphene/carbon nanotubes (NGR–NCNTs) nanocomposite was employed into the study of the electrochemical sensor via electrodeposition for the first time. The morphology and structure of NGR–NCNTs nanocomposite were investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. Meanwhile, the electrochemical performance of the glassy carbon electrode (GCE) modified with electrodeposited NGR–NCNTs (ENGR–NCNTs/GCE) towards caffeine (CAF) and vanillin (VAN) determination was demonstrated by cyclic voltammetry (CV) and square wave voltammetry (SWV). Under optimal condition, ENGR–NCNTs/GCE exhibited a wide linearity of 0.06–50 μM for CAF and 0.01–10 μM for VAN with detection limits of 0.02 μM and 3.3 × 10 −3 μM, respectively. Furthermore, the application of the proposed sensor in food products was proven to be practical and reliable. The desirable results show that the ENGR–NCNTs nanocomposite has promising potential in electrocatalytic biosensor application

  4. Simultaneous Spectrophotometric Determination of Valsartan and ...

    African Journals Online (AJOL)

    Purpose: To develop a direct, simple and extraction-free spectrophotometric method for the simultaneous estimation of valsartan and ezetimibe in pharmaceuticals. Methods: A spectrophotometric method for the determination of valsartan and ezetimibe was developed using acidic dyes, namely, bromophenol blue (BPB) ...

  5. Amplified nanostructure electrochemical sensor for simultaneous determination of captopril, acetaminophen, tyrosine and hydrochlorothiazide

    Energy Technology Data Exchange (ETDEWEB)

    Karimi-Maleh, Hassan, E-mail: h.karimi.maleh@gmail.com [Department of Chemistry, Graduate University of Advanced Technology, Kerman (Iran, Islamic Republic of); Ganjali, Mohammad R.; Norouzi, Parviz; Bananezhad, Asma [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of)

    2017-04-01

    A novel nanomaterial-based voltammetric sensor has been developed for use a highly sensitive tool for the simultaneous determination of captopril (CA), acetaminophen (AC), tyrosine (TY) and hydrochlorothiazide (HCTZ). The device is based on the application of NiO/CNTs and (2-(3,4-dihydroxyphenethyl)isoindoline-1,3-dione) (DPID) to modify carbon paste electrodes. The NiO/CNTs nanocomposite was synthesized through a direct chemical precipitation approach and was characterized with X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The NiO/CNTs/DPID/CPEs were found to facilitate the analysis of CA, AC, TY and HCTZ in the concentration ranges of 0.07–200.0, 0.8–550.0, 5.0–750.0 and 10.0–600.0 μM with the respective detection limits of 9.0 nM, 0.3 μM, 1.0 μM and 5.0 μM. The developed NiO/CNTs/DPID/CPEs were used for the determination of the mentioned analytes in pharmaceutical and biological real samples. - Graphical abstract: In this study a novel sensor based on NiO/CNTs and (2-(3,4-dihydroxyphenethyl)isoindoline-1,3-dione) (DPID) modified carbon paste electrode fabricated for simultaneous determination of captopril, acetaminophen, tyrosine and hydrochlorothiazide for the first time. - Highlights: • Fabrication of NiO/CNTs and new catechol derivative modified carbon paste electrode • Good ability of proposed sensor for biological and pharmaceutical analysis • Simultaneous determination captopril, acetaminophen, tyrosine and hydrochlorothiazide.

  6. Simultaneous Determination of Amlodipine and Valsartan

    OpenAIRE

    Mohamed, Nashwah Gadallah

    2011-01-01

    A spectrophotometric method was developed for simultaneous determination of amlodipine (Aml) and valsartan (Val) without previous separation. In this method amlodipine in methanolic solution was determined using zero order UV spectrophotometry by measuring its absorbency at 360.5 nm without any interference from valsartan. Valsartan spectrum in zero order is totally overlapped with that of amlodipine. First, second and third derivative could not resolve the overlapped peaks. The first derivat...

  7. Development and validation of a sensitive LC-MS-MS method for the simultaneous determination of multicomponent contents in artificial Calculus Bovis.

    Science.gov (United States)

    Peng, Can; Tian, Jixin; Lv, Mengying; Huang, Yin; Tian, Yuan; Zhang, Zunjian

    2014-02-01

    Artificial Calculus Bovis is a major substitute in clinical treatment for Niuhuang, a widely used, efficacious but rare traditional Chinese medicine. However, its chemical structures and the physicochemical properties of its components are complicated, which causes difficulty in establishing a set of effective and comprehensive methods for its identification and quality control. In this study, a simple, sensitive and reliable liquid chromatography-tandem mass spectrometry method was successfully developed and validated for the simultaneous determination of bilirubin, taurine and major bile acids (including six unconjugated bile acids, two glycine-conjugated bile acids and three taurine-conjugated bile acids) in artificial Calculus Bovis using a Zorbax SB-C18 column with a gradient elution of methanol and 10 mmol/L ammonium acetate in aqueous solution (adjusted to pH 3.0 with formic acid). The mass spectra were obtained in the negative ion mode using dehydrocholic acid as the internal standard. The content of each analyte in artificial Calculus Bovis was determined by monitoring specific ion pairs in the selected reaction monitoring mode. All analytes demonstrated perfect linearity (r(2) > 0.994) in a wide dynamic range, and 10 batches of samples from different sources were further analyzed. This study provided a comprehensive method for the quality control of artificial Calculus Bovis.

  8. Simultaneous determination of radium and uranium in soil

    International Nuclear Information System (INIS)

    Yamamoto, Takashi; Yuki, Eiji; Ishida, Tatsuo

    1977-01-01

    Radium and uranium contents in soil are the fundamental indexes for natural radioactivity. In this connection, the simultaneous determination of Ra and U has been studied. To a soil sample, 133 Ba is added and the mixture is dried. It is decomposed with sulfuric and nitric acids. Then a Ba-carrier is added, and the insoluble residue (Ra analysis sample) and the solution (U analysis sample) are obtained for simultaneous determination of Ra and U. The rates of recovery of Ra and U in soil are both over 90%. (Mori, K.)

  9. Simultaneous velocity and pressure quantification using pressure-sensitive flow tracers in air

    Science.gov (United States)

    Zhang, Peng; Peterson, Sean; Porfiri, Maurizio

    2017-11-01

    Particle-based measurement techniques for assessing the velocity field of a fluid have advanced rapidly over the past two decades. Full-field pressure measurement techniques have remained elusive, however. In this work, we aim to demonstrate the possibility of direct simultaneous planar velocity and pressure measurement of a high speed aerodynamic flow by employing novel pressure-sensitive tracer particles for particle image velocimetry (PIV). Specifically, the velocity and pressure variations of an airflow through a converging-diverging channel are studied. Polystyrene microparticles embedded with a pressure-sensitive phosphorescent dye-platinum octaethylporphyrin (PtOEP)-are used as seeding particles. Due to the oxygen quenching effect, the emission lifetime of PtOEP is highly sensitive to the oxygen concentration, that is, the partial pressure of oxygen, in the air. Since the partial pressure of oxygen is linearly proportional to the air pressure, we can determine the air pressure through the phosphorescence emission lifetime of the dye. The velocity field is instead obtained using traditional PIV methods. The particles have a pressure resolution on the order of 1 kPa, which may be improved by optimizing the particle size and dye concentration to suit specific flow scenarios. This work was supported by the National Science Foundation under Grant Number CBET-1332204.

  10. Simultaneous determination of ascorbic acid, dopamine and uric acid using high-performance screen-printed graphene electrode.

    Science.gov (United States)

    Ping, Jianfeng; Wu, Jian; Wang, Yixian; Ying, Yibin

    2012-04-15

    A disposable and sensitive screen-printed electrode using an ink containing graphene was developed. This electrode combined the advantages of graphene and the disposable characteristic of electrode, which possessed wide potential window, low background current and fast electron transfer kinetics. Compared with the electrodes made from other inks, screen-printed graphene electrode (SPGNE) showed excellent electrocatalytic activity for the oxidation of ascorbic acid (AA), dopamine (DA), and uric acid (UA). Three well-defined sharp and fully resolved anodic peaks were found at the developed electrode. Differential pulse voltammetry was used to simultaneous determination of AA, DA, and UA in their ternary mixture. In the co-existence system of these three species, the linear response ranges for the determination of AA, DA, and UA were 4.0-4500 μM, 0.5-2000 μM, and 0.8-2500 μM, respectively. The detection limits (S/N=3) were found to be 0.95 μM, 0.12 μM, and 0.20 μM for the determination of AA, DA, and UA, respectively. Furthermore, the SPGNE displayed high reproducibility and stability for these species determination. The feasibility of the developed electrode for real sample analysis was investigated. Results showed that the SPGNE could be used as a sensitive and selective sensor for simultaneous determination of AA, DA, and UA in biological samples, which may provide a promising alternative in routine sensing applications. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Efficient Noninferiority Testing Procedures for Simultaneously Assessing Sensitivity and Specificity of Two Diagnostic Tests

    Directory of Open Access Journals (Sweden)

    Guogen Shan

    2015-01-01

    Full Text Available Sensitivity and specificity are often used to assess the performance of a diagnostic test with binary outcomes. Wald-type test statistics have been proposed for testing sensitivity and specificity individually. In the presence of a gold standard, simultaneous comparison between two diagnostic tests for noninferiority of sensitivity and specificity based on an asymptotic approach has been studied by Chen et al. (2003. However, the asymptotic approach may suffer from unsatisfactory type I error control as observed from many studies, especially in small to medium sample settings. In this paper, we compare three unconditional approaches for simultaneously testing sensitivity and specificity. They are approaches based on estimation, maximization, and a combination of estimation and maximization. Although the estimation approach does not guarantee type I error, it has satisfactory performance with regard to type I error control. The other two unconditional approaches are exact. The approach based on estimation and maximization is generally more powerful than the approach based on maximization.

  12. Rapid and sensitive approach to simultaneous detection of genomes of hepatitis A, B, C, D and E viruses.

    Science.gov (United States)

    Kodani, Maja; Mixson-Hayden, Tonya; Drobeniuc, Jan; Kamili, Saleem

    2014-10-01

    Five viruses have been etiologically associated with viral hepatitis. Nucleic acid testing (NAT) remains the gold standard for diagnosis of viremic stages of infection. NAT methodologies have been developed for all hepatitis viruses; however, a NAT-based assay that can simultaneously detect all five viruses is not available. We designed TaqMan card-based assays for detection of HAV RNA, HBV DNA, HCV RNA, HDV RNA and HEV RNA. The performances of individual assays were evaluated on TaqMan Array Cards (TAC) for detecting five viral genomes simultaneously. Sensitivity and specificity were determined by testing 329 NAT-tested clinical specimens. All NAT-positive samples for HCV (n = 32), HDV (n = 28) and HEV (n = 14) were also found positive in TAC (sensitivity, 100%). Forty-three of 46 HAV-NAT positive samples were also positive in TAC (sensitivity, 94%), while 36 of 39 HBV-NAT positive samples were positive (sensitivity, 92%). No false-positives were detected for HBV (n = 32), HCV (n = 36), HDV (n = 30), and HEV (n = 31) NAT-negative samples (specificity 100%), while 38 of 41 HAV-NAT negative samples were negative by TAC (specificity 93%). TAC assay was concordant with corresponding individual NATs for hepatitis A-E viral genomes and can be used for their detection simultaneously. The TAC assay has potential for use in hepatitis surveillance, for screening of donor specimens and in outbreak situations. Wider availability of TAC-ready assays may allow for customized assays, for improving acute jaundice surveillance and for other purposes for which there is need to identify multiple pathogens rapidly. Published by Elsevier B.V.

  13. A method for simultaneous determination of wear-resistance of structurally identical machine parts with mutual friction

    International Nuclear Information System (INIS)

    Valigura, V.; Volyn'ski, A.

    1979-01-01

    There are mechanisms in the technique, boundary state of separate parts of which is determined by the process of wear of three elements of the mechanism, made of the same material (for example antifriction bearings). The main concept of wear determination in the case of such a mechanism is to conduct measurements by means of simultaneous application of three different methods, for example: the method of roentgen-fluorescence; the tracer technique with application of activation by means of irradiation by different elementary particles, practically by means of neutrons and protons; the method of artifical bases application. In the paper the method is presented having been developed in the Institute of Working Machines of the Poznan Polytechnic. This method of simultaneous investigation in the wear process of bearing rings, inner and outer, and rolling elements of roller bearings. All these elements of bearings are made of LX-15 steel. The method developed, permits to determine the wear sufficient for practical purposes sensitivity [ru

  14. Sensitization of uranium fluorescence using 2,6-pyridinedicarboxylic acid: Application for the determination of uranium in the presence of lanthanides

    International Nuclear Information System (INIS)

    Maji, S.; Viswanathan, K.S.

    2009-01-01

    The 2,6-pyridinedicarboxylic acid (PDA) has been shown to efficiently sensitize and enhance the fluorescence of uranium in aqueous medium. Interestingly, this ligand stabilizes the UO 2 2+ species, which without the ligand is known to be in a negligible concentration, in aqueous medium at pH 6. The ligand sensitized enhancement of UO 2 2+ fluorescence by PDA, provides an analytical tool for the determination of uranium at trace levels, in aqueous medium. Furthermore, PDA is also known to enhance the fluorescence of lanthanides; consequently, the simultaneous determination of uranium and lanthanides, using PDA as a fluorescence sensitizing agent, becomes a possibility, which has been demonstrated in this work. We have shown that the use of PDA yields detection limits of 2.2x10 -7 M for UO 2 2+ , 1x10 -8 M for Tb 3+ and 5x10 -9 M for Eu 3+ in the simultaneous determination of these analytes.

  15. Simultaneous determination of inorganic mercury and methylmercury compounds in natural waters

    Energy Technology Data Exchange (ETDEWEB)

    Logar, Martina; Horvat, Milena [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia); Akagi, Hirokatsu [National Institute for Minamata Disease, 4058-18 Hama, Minamata, Kumamoto 867-0008 (Japan); Pihlar, Boris [Faculty of Chemistry and Chemical Technology, University of Ljubljana, Askerceva 5, 1000 Ljubljana (Slovenia)

    2002-11-01

    The purpose of the present work was to develop a simple, rapid, sensitive and accurate method for the simultaneous determination of inorganic mercury (Hg{sup 2+}) and monomethylmercury compounds (MeHg) in natural water samples at the pg L{sup -1} level. The method is based on the simultaneous extraction of MeHg and Hg{sup 2+}dithizonates into an organic solvent (toluene) after acidification of about 300 mL of a water sample, followed by back extraction into an aqueous solution of Na {sub 2}S, removal of H {sub 2}S by purging with N {sub 2}, subsequent ethylation with sodium tetraethylborate, room temperature precollection on Tenax, isothermal gas chromatographic separation (GC), pyrolysis and cold vapour atomic fluorescence spectrometric detection (CV AFS) of mercury. The limit of detection calculated on the basis of three times the standard deviation of the blank was about 0.006 ng L {sup -1} for MeHg and 0.06 ng L {sup -1} for Hg {sup 2+}when 300 mL of water was analysed. The repeatability of the results was about 5% for MeHg and 10% for Hg {sup 2+}. Recoveries were 90-110% for both species. (orig.)

  16. Self-powered detectors sensitivity determination

    International Nuclear Information System (INIS)

    Surkov, V.; Soares, A.J.

    1994-01-01

    The determination of the initial sensitivity of Self Powered Detectors (SPDs) was performed. Measurements of thermal, epithermal and to gamma flux sensitivities were made with Vanadium, Cobalt, Rhodium, Silver and Platinum SPDs and, when possible, the values are compared with the ones from the existing literature. The determination of neutron sensitivity was realized using the IEA-R1 Reactor from IPEN. The thermal and epithermal neutron flux were determined with bare and Cadmium covered activation foils. (GOLD). (author)

  17. Simultaneous determination of ten compounds in two main ...

    African Journals Online (AJOL)

    Simultaneous determination of ten compounds in two main medicinal plant parts of Tibetan herb, Pterocephalus hookeri (CB Clarke) Höeck, by ultra-high performance liquid chromatography-photodiode array.

  18. Simultaneous Determination of Seven Constituents in Herbal ...

    African Journals Online (AJOL)

    Simultaneous Determination of Seven Constituents in Herbal Prescription Jaeumganghwa-Tang Using HPLC-PDA. CS Seo, JH Kim, HK Shin. Abstract. A simple and accurate high-performance liquid chromatographic method was applied to the quantitative analysis of seven components of the traditional herbal prescription ...

  19. Simultaneous determination of a binary mixture: kinetic method for determination of uranium and vanadium

    International Nuclear Information System (INIS)

    Jianhua, W.; Ronghuan, H.

    1993-01-01

    A kinetic method for simultaneous determination of a binary mixture is proposed, and a procedure for simultaneous determination of uranium (IV) and vanadium (IV) is established based on their inductive effect on chromium (VI)-iodide redox reaction in a weak acidic medium. The reaction was monitored by FIA-spectrophotometry using the I 3 - -starch complex as indicator. The calibration graphs are linear for uranium (IV) and vanadium (IV) within the range of 0 ∼ 3.6 μg/ml and 0 ∼ 2.5 μg/ml respectively. Most foreign ions, except for iron (II) and antimony (III), do not interfere with the determination. The uranium and vanadium content in different samples was determined, and the results were satisfactory. (author). 2 tabs., 2 figs., 9 refs

  20. Simultaneous Determination of Hydroquinone and Catechol by Poly (L-methionine Coated Hydroxyl Multiwalled Carbon Nanotube Film

    Directory of Open Access Journals (Sweden)

    Ying Zhang

    2014-07-01

    Full Text Available A simply and high selectively electrochemical method has been developed for the simultaneous determination of hydroquinone and catechol at a glassy carbon electrode modified with the poly L-methionine/multiwall carbon nanotubes, which significantly increased the reversible electrochemical reaction. The electrochemical behavior of catechol and hydroquinone at the modified electrode was studied by cyclic voltammetry and differential pulse voltammetry. The presence of hydroxyl MWCNTs in the composite film enhances the surface coverage concentration of poly L- methionine/multiwall carbon nanotubes. The results suggest that pH=6 is the optimum acidity condition for the selective and simultaneous determination of catechol and hydroquinone. Under the optimized condition, the response peak currents of the modified electrodes were linear over ranges of 8.0´10-7~2.0´10-4 mol/L (R2=0.997 for hydroquinone and 8.0´10-7~2.0´10-4, R2=0.997 for catechol. The sensor also exhibited good sensitivity with the detection limit of 8.0´10-8 mol/L and 1.0´10- 7 mol/L for hydroquinone and catechol, respectively. This study provides a new kind of composite modified electrode for electrochemical sensors with good selectivity and strong anti- interference. It has been applied to simultaneous determination of hydroquinone and catechol in water sample with simplicity and high selectivity.

  1. [Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

    Science.gov (United States)

    Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

    2014-05-01

    A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

  2. Simultaneous Determination of Cyclosporine A, Tacrolimus, Sirolimus, and Everolimus in Whole-Blood Samples by LC-MS/MS

    Directory of Open Access Journals (Sweden)

    Mustafa Karapirli

    2012-01-01

    Full Text Available Objectives. Cyclosporine A (CyA, tacrolimus (TRL, sirolimus (SIR, and everolimus (RAD are immunosuppressive drugs frequently used in organ transplantation. Our aim was to confirm a robust sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS method for determination of CyA, TRL, SIR, and RAD in whole-blood samples. Materials and Methods. We used an integrated online solid-phase extraction-LC-MS/MS system and atmospheric pressure ionization tandem mass spectrometry (API-MS/MS in the multiple reaction monitoring (MRM detection mode. CyA, TRL, SIR, and RAD were simultaneously analyzed in whole blood treated with precipitation reagent taken from transplant patients. Results. System performance parameters were suitable for using this method as a high-throughput technique in clinical practice. The high concentration of one analyte in the sample did not affect the concentration of other analytes. Total analytical time was 2.5 min, and retention times of all analytes were shorter than 2 minutes. Conclusion. This LC-MS/MS method can be preferable for therapeutic drug monitoring of these immunosuppressive drugs (CyA, TRL, SRL, and RAD in whole blood. Sample preparation was too short and simple in this method, and it permits robust, rapid, sensitive, selective, and simultaneous determination of these drugs.

  3. Sensitization of uranium fluorescence using 2,6-pyridinedicarboxylic acid: Application for the determination of uranium in the presence of lanthanides

    Energy Technology Data Exchange (ETDEWEB)

    Maji, S. [Materials Chemistry Division, Chemistry Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India); Viswanathan, K.S., E-mail: vish@igcar.gov.i [Materials Chemistry Division, Chemistry Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India)

    2009-11-15

    The 2,6-pyridinedicarboxylic acid (PDA) has been shown to efficiently sensitize and enhance the fluorescence of uranium in aqueous medium. Interestingly, this ligand stabilizes the UO{sub 2}{sup 2+} species, which without the ligand is known to be in a negligible concentration, in aqueous medium at pH 6. The ligand sensitized enhancement of UO{sub 2}{sup 2+} fluorescence by PDA, provides an analytical tool for the determination of uranium at trace levels, in aqueous medium. Furthermore, PDA is also known to enhance the fluorescence of lanthanides; consequently, the simultaneous determination of uranium and lanthanides, using PDA as a fluorescence sensitizing agent, becomes a possibility, which has been demonstrated in this work. We have shown that the use of PDA yields detection limits of 2.2x10{sup -7} M for UO{sub 2}{sup 2+}, 1x10{sup -8} M for Tb{sup 3+} and 5x10{sup -9} M for Eu{sup 3+} in the simultaneous determination of these analytes.

  4. Simultaneous determination of rutin and ascorbic acid in a sequential injection lab-at-valve system.

    Science.gov (United States)

    Al-Shwaiyat, Mohammed Khair E A; Miekh, Yuliia V; Denisenko, Tatyana A; Vishnikin, Andriy B; Andruch, Vasil; Bazel, Yaroslav R

    2018-02-05

    A green, simple, accurate and highly sensitive sequential injection lab-at-valve procedure has been developed for the simultaneous determination of ascorbic acid (Asc) and rutin using 18-molybdo-2-phosphate Wells-Dawson heteropoly anion (18-MPA). The method is based on the dependence of the reaction rate between 18-MPA and reducing agents on the solution pH. Only Asc is capable of interacting with 18-MPA at pH 4.7, while at pH 7.4 the reaction with both Asc and rutin proceeds simultaneously. In order to improve the precision and sensitivity of the analysis, to minimize reagent consumption and to remove the Schlieren effect, the manifold for the sequential injection analysis was supplemented with external reaction chamber, and the reaction mixture was segmented. By the reduction of 18-MPA with reducing agents one- and two-electron heteropoly blues are formed. The fraction of one-electron heteropoly blue increases at low concentrations of the reducer. Measurement of the absorbance at a wavelength corresponding to the isobestic point allows strictly linear calibration graphs to be obtained. The calibration curves were linear in the concentration ranges of 0.3-24mgL -1 and 0.2-14mgL -1 with detection limits of 0.13mgL -1 and 0.09mgL -1 for rutin and Asc, respectively. The determination of rutin was possible in the presence of up to a 20-fold molar excess of Asc. The method was applied to the determination of Asc and rutin in ascorutin tablets with acceptable accuracy and precision (1-2%). Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Sensitivity of decomposition rates of soil organic matter with respect to simultaneous changes in temperature and moisture

    Science.gov (United States)

    Sierra, Carlos A.; Trumbore, Susan E.; Davidson, Eric A.; Vicca, Sara; Janssens, I.

    2015-03-01

    The sensitivity of soil organic matter decomposition to global environmental change is a topic of prominent relevance for the global carbon cycle. Decomposition depends on multiple factors that are being altered simultaneously as a result of global environmental change; therefore, it is important to study the sensitivity of the rates of soil organic matter decomposition with respect to multiple and interacting drivers. In this manuscript, we present an analysis of the potential response of decomposition rates to simultaneous changes in temperature and moisture. To address this problem, we first present a theoretical framework to study the sensitivity of soil organic matter decomposition when multiple driving factors change simultaneously. We then apply this framework to models and data at different levels of abstraction: (1) to a mechanistic model that addresses the limitation of enzyme activity by simultaneous effects of temperature and soil water content, the latter controlling substrate supply and oxygen concentration for microbial activity; (2) to different mathematical functions used to represent temperature and moisture effects on decomposition in biogeochemical models. To contrast model predictions at these two levels of organization, we compiled different data sets of observed responses in field and laboratory studies. Then we applied our conceptual framework to: (3) observations of heterotrophic respiration at the ecosystem level; (4) laboratory experiments looking at the response of heterotrophic respiration to independent changes in moisture and temperature; and (5) ecosystem-level experiments manipulating soil temperature and water content simultaneously.

  6. Precise simultaneous determination of zirconium and hafnium in silicate rocks, meteorites and lunar samples. [Neutron reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, P A; Garg, A N; Ehmann, W D [Kentucky Univ., Lexington (USA). Dept. of Chemistry

    1977-01-01

    A precise, sensitive and rapid analytical technique has been developed for the simultaneous determination of Zr and Hf in natural silicate matrices. The technique is based on radiochemical neutron activation analysis and employs a rapid fusion dissolution of the sample and simultaneous precipitation of the Zr-Hf pair with p-hydroxybenzene arsenic acid in an acidic medium. The indicator radionuclides, /sup 95/Zr and /sup 181/Hf, are counted and the /sup 95/Zr activity is corrected for the contribution from U fission. The chemical yields of the radiochemical separation are based on Hf carrier. The yield is determined by reactivation of the processed samples and standards with a /sup 252/Cf isotopic neutron source and by counting the 18.6 sec half-life sup(179m)Hf. The RNAA procedure for Zr and Hf has been shown to be precise and accurate for natural silicate samples, based on replicate analyses of samples containing Zr in the range of 1 ..mu..g/g to over 600 ..mu..g/g. The procedure is relatively rapid with a total chemical processing time of approximately 3 hours. At least 4 samples are processed simultaneously. Ten additional elements (Fe, Cr, Co, Sc, Eu, La, Lu, Ce, Th and Tb) can be determined by direct Ge(Li) spectrometry (INAA) on the samples prior to dissolution for the RNAA determination of Zr and Hf. Corrections for the U fission contribution can be made on the basis of the known U content or from the INAA Th content, based on the relatively constant natural Th/U ratio.

  7. A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

    Science.gov (United States)

    Ball, J.W.; Nordstrom, D. Kirk

    1994-01-01

    Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of

  8. Simultaneous Determination of Flavonols and Terpene Lactones in ...

    African Journals Online (AJOL)

    Purpose: To develop an ultra-performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS) method for the simultaneous determination of 7 major components of Ginkgo leaf (kaempferol, quercetin, isorhamnetin, ginkgolides A, ginkgolides B, ginkgolides C and bilobalide) in dog plasma. Methods: Beagle ...

  9. Simultaneous Determination of Fifteen Constituents of Jitai Tablet Using Ultra High-Performance Liquid Chromatography Coupled with Triple Quadrupole Electrospray Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Shuping Wang

    2014-01-01

    Full Text Available An ultra-high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS method was developed for simultaneous determination of fifteen constituents in Jitai tablet (JTT, a complex Traditional Chinese Medicine prescription (TCMP used in treating opiate addiction. Benefitting from a small particle size (1.8 µm C18 column, accelerated analysis with satisfactory resolution, sensitivity and selectivity were achieved in a single run within 7 min with linear gradient elution of acetonitrile-0.1% (v/v formic acid in water. The analytical signal was obtained by multiple reaction monitoring transitions via electrospray ionization source operating in both positive and negative ionization mode. The approach was validated for linearity, sensitivity, precision, repeatability, stability and recovery. All analytes showed good linearity over a wide concentration range (r > 0.99. The method limits ranged from 0.03 ng/mL to 19.35 ng/mL which are sensitive enough for quality control studies. The developed method was successfully applied to the simultaneous determination of fifteen constituents in JTT. In conclusion, our experimental results demonstrate that UHPLC-ESI-MS/MS is a useful approach for the overall quality assessment of complex TCMPs.

  10. Simultaneous Determination of Two Isomers of Asarone in Piper ...

    African Journals Online (AJOL)

    Simultaneous Determination of Two Isomers of Asarone in Piper sarmentosum Roxburgh (Piperaceae) Extracts using Different Chromatographic Columns. Mohd Shahrul Ridzuan Hamil, Abdul Hakeem Memon, Amin Malik Shah Abdul Majid, Zhari Ismail ...

  11. Simultaneous spectrophotometric determination of binary mixtures of surfactants using continuous wavelet transformation

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Nematollahi, Davood; Madrakian, Tayyebeh; Abbasi-Tarighat, Maryam; Hajihadi, Mitra

    2009-01-01

    This work presents a simple, rapid, and novel method for simultaneous determination of binary mixtures of some surfactants using continuous wavelet transformation. The method is based on the difference in the effect of surfactants Cetyltrimethylammoniumbromide (CTAB), dodecyl trimethylammonium bromide (DTAB), cetylpyridinium bromide (CPB) and TritonX-100 (TX-100) on the absorption spectra of complex of Beryllium with Chrome Azurol S (CAS) at pH 5.4. Binary mixtures of CTAB-DTAB, DTAB-CPB and CTAB-TX-100 were analyzed without prior separation steps. Different mother wavelets from the family of continuous wavelet transforms were selected and applied under the optimal conditions for simultaneous determinations. The proposed methods, under the working conditions, were successfully applied to simultaneous determination of surfactants in hair conditioner and mouthwash samples.

  12. Dual-mode gradient HPLC procedure for the simultaneous determination of chloroquine and proguanil.

    Science.gov (United States)

    Paci, A; Caire-Maurisier, A-M; Rieutord, A; Brion, F; Clair, P

    2002-01-01

    In order to assay the antipaludic capsule of the Service de Santé des Armées (SSA), that contains two antimalarial drugs, i.e. chloroquine sulfate (CQS, cp1) and proguanil hydrochloride (PGH, cp5), a HPLC procedure was developed. A reversed-phase ion-pair high-performance liquid chromatography (HPLC) method with an ultraviolet detection at 254 nm was set up and validated. Elution system includes programming of both organic concentration and flow-rate known as 'dual-mode gradient'. This method allows the simultaneous determination of both active compounds and separation of four process related substances. The method is simple, rapid, selective and accurate, and the precision is good with an inter- and intra-assay of <2%. The sensitivity is particularly suitable for pharmaceutical quality control.

  13. Simultaneous determination of boron, carbon and nitrogen in silicon by deuteron activation analysis

    International Nuclear Information System (INIS)

    He, Shiyu; Wang, Yinsong; Jin, Baikang; Hua, Zhifen; Zhao, Kaihua

    1984-01-01

    The paper describes simultaneous determination of trace quantities of B, C and N in semiconductor silicon by nuclear reaction of 10 B(d, n) 11 C(T 1/2 = 20.3 min), 11 B(d, 2n) 11 C, 12 C(d, n) 13 N(T 1/2 = 9.96 min) and 14 N(d, n) 15 O(T 1/2 = 2.03 min) with deuterons from a 1.2 m cyclotron in our institute. An inert-gas fusion technique is adopted for rapid radiochemical separation after irradiation of the samples. 11 C, 13 N and 15 O are absorbed in ascarite 5A molecular sieve cooled in liquid nitrogen and Hopcalite reagent at a temperature of 650 deg C respectively. Positron Annihilation events of each produced nucleus are counted by a γ - γ coincidence measuring system. B, C and N contents of about several ten parts per billion in silicon are then calculated simultaneously by a relatively quantitative method. Relative standard deviation for C, B and N are less than +-50% respectively. This method is simple, rapid and sensitive for estimating light element content in silicon material. (author)

  14. Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

    International Nuclear Information System (INIS)

    Ba Xi; Luo Liqiang; Ding Yaping; Zhang Zhen; Chu Yuliang; Wang Bijun; Ouyang Xiaoqian

    2012-01-01

    Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 μM G, 50.0 μM A, 100.0 μM T and 100.0 μM C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: ► The sensor exhibited well-separated peaks and low detection limit. ► The sensor possesses high sensitivity and wide linear range. ► The sensor was used for simultaneous detection of G, A, T and C successfully. ► The sensor was applied in a fish sperm DNA sample with satisfactory results. ► The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

  15. Application of adsorptive stripping voltammetry to the simultaneous determination of bismuth and copper in the presence of nuclear fast red

    International Nuclear Information System (INIS)

    Gholivand, M.B.; Romiani, A.A.

    2006-01-01

    A sensitive and selective method for the simultaneous determination of copper and bismuth by adsorptive stripping was developed using nuclear fast red (2-anthracenesulfonic acid, 4-amino-9,10-dihydro-1,3-dihydroxy-9,10-dioxo-, monosodium salt) as selective complexing agent onto hanging mercury drop electrode. In a single scan both metals gave peaks that were distinctly separated by 85 mV allowing their determination in the presence of each other. Optimal analytical conditions were found to be: nuclear fast red concentration of 80 μM, pH of 2.8 and adsorptive potential of -300 mV versus Ag/AgCl. With accumulation time of 180 s the peaks currents are proportional to concentration of copper and bismuth over the 1-100 and 5-60 ng mL -1 range with detection limits of 0.2 and 1.2 ng mL -1 , respectively. The procedure was applied to simultaneous determination of copper and bismuth in some real samples

  16. Simultaneous determination of oxygen and cadmium in cadmium and cadmium compounds

    International Nuclear Information System (INIS)

    Imaeda, K.; Kuriki, T.; Ohsawa, K.; Ishii, Y.

    1977-01-01

    Cadmium and its compounds were analysed for oxygen and cadmium by a modification of the Schutze-Unterzaucher method. Oxygen in some compounds such as cadmium oxide, nitrate and sulphate could not be determined by the usual method. The method of adding carbon was employed for the determination of total oxygen. Total oxygen could be determined by the addition of 5 mg of carbon to a sample boat and heating at 950 0 . The determination was also carried out by addition of naphthalene (2 mg). It was found that the cadmium powder and cadmium flake used contained ca. 1 and 0.15% oxygen, respectively. Oxygen and cadmium in cadmium and its compounds were simultaneously determined by the addition of 2 mg of naphthalene. Cadmium was determined colorimetrically by use of glyoxal-bis-(2-hydroxyanil). Oxygen and cadmium in the samples could be determined simultaneously with an average error of -0.02 and -0.22%, respectively. (author)

  17. Simultaneous Spectrophotometric Determination of Copper, Nickel, and Zinc Using 1-(2-Thiazolylazo)-2-Naphthol in the Presence of Triton X-100 Using Chemometric Methods

    International Nuclear Information System (INIS)

    Low, Kah Hin; Zain, Sharifuddin Md; Abas, Mhd. Radzi; Misran, Misni; Mohd, Mustafa Ali

    2009-01-01

    Multivariate models were developed for the simultaneous spectrophotometric determination of copper (II), nickel (II) and zinc (II) in water with 1-(2-thiazolylazo)-2-naphthol as chromogenic reagent in the presence of Triton X-100. To overcome the drawback of spectral interferences, principal component regression (PCR) and partial least square (PLS) multivariate calibration approaches were applied. Performances were validated with several test sets, and their results were then compared. In general, no significant difference in analytical performance between PLS and PCR models. The root mean square error of prediction (RMSEP) using three components for Cu 2+ , Ni 2+ and Zn 2+ were 0.018, 0.010, 0.011 ppm, respectively. Figures of merit such as sensitivity, analytical sensitivity, limit of detection (LOD) were also estimated. High reliability was achieved when the proposed procedure was applied to simultaneous determination of Cu 2+ , Ni 2+ and Zn 2+ in synthetic mixture and tap water

  18. Simultaneous determination of plutonium and uranium in environmental samples

    International Nuclear Information System (INIS)

    Jiao Shufen

    1993-01-01

    Plutonium and uranium in a plant sample ash was simultaneously determined by using anion exchange resin columns, and concentrated hydrochloric acid and nitric acid. At the final stage of the determination of the nuclides, each of them was electrodeposited together with a little amount of molybdenum carrier onto a stainless steel plate and measured by α-ray spectrometer. The recoveries of uranium and plutonium from the plant samples determined by adding internal standard 236 Pu which was 100% and 63%, respectively

  19. A Simple and Sensitive RP-UPLC Method for the Simultaneous Determination of N-Hydroxybenzotriazole, Cinchonidine and 1,3-Dicyclohexyl Urea Contents in Fosinopril Sodium Drug Substance

    Directory of Open Access Journals (Sweden)

    M. Narendra Kumar

    2012-01-01

    Full Text Available A simple and sensitive reverse phase ultra performance liquid chromatography (RP-UPLC method has been developed, optimized and validated for the simultaneous determination of N-Hydroxybenzotriazole (HOBt, Cinchonidine and 1,3-Dicyclohexyl urea (DCU contents at low levels in fosinopril sodium drug substance. Efficient chromatographic separation was achieved on Acquity UPLC HSS C18 column, 100 mm long with 2.1 mm i.d., 1.8 µm particle diameter, thermo stated at 30°C. Gradient elution involving binary mixture of potassium dihydrogen orthophosphate (0.01M, pH:3.0±0.05 with ortho-phosphoric acid and acetonitrile at a flow rate of 0.10 mL min-1 has been used. The analytes were monitored by photodiode array (PDA detector set at 205 nm. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolysis, thermal and humidity degradation. The method was validated for specificity, sensitivity, linearity, precision, accuracy and solution stability. The limit of detection (LOD and limit of quantification (LOQ for HOBt, Cinchonidine and DCU were in the range of 0.85-3.52 ppm and 2.57-10.67 ppm, respectively. The average recoveries for HOBt, Cinchonidine and DCU are in the range of 98.1% to 102.6%. The method can be used for the routine quality control analysis of fosinopril sodium drug substance.

  20. Radioenzymatic simultaneous determination of epinephrine and norepinephrine in plasma

    International Nuclear Information System (INIS)

    Mueller, T.

    1978-01-01

    The high-pressure liquid chromatography (= HPLC) was used in simultaneous determinations of a few pg epinephrine and norepinephrine. This separation procedure improves the efficiency when compared with the conventional thin-layer chromatographic methods (TLC) and allows routine assays in plasma. (orig.) [de

  1. Electrochemical behaviors and simultaneous determination of guanine and adenine based on graphene–ionic liquid–chitosan composite film modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Niu Xiuli; Yang Wu; Ren Jie; Guo Hao; Long Shijia; Chen Jiaojiao; Gao Jinzhang

    2012-01-01

    Highlights: ► This work developed a novel electrochemical biosensors for guanine and adenine detection simultaneously. ► A disposable electrode based on graphene sheets, ionic liquid and chitosan was proposed. ► The presented method was also applied to simultaneous determination of guanine and adenine in denatured DNA samples with satisfying results. ► Easy fabrication, high sensitivity, excellent reproducibility and long-term stability. - Abstract: A graphene sheets (GS), ionic liquid (IL) and chitosan (CS) modified electrode was fabricated and the modified electrode displayed excellent electrochemical catalytic activities toward guanine and adenine. The transfer electron number (n) and the charge transfer coefficient (α) were calculated with the result as n = 2, α = 0.58 for guanine, and n = 2, α = 0.51 for adenine, which indicated the electrochemical oxidation of guanine and adenine on GS/IL/CS modified electrode was a two-electron and two-proton process. The oxidation overpotentials of guanine and adenine were decreased significantly compared with those obtained at the bare glassy carbon electrode and multi-walled carbon nanotubes modified electrode. The modified electrode exhibited good analytical performance and was successfully applied for individual and simultaneous determination of guanine and adenine. Low detection limits of 0.75 μM for guanine and 0.45 μM for adenine were obtained, with the linear calibration curves over the concentration range 2.5–150 μM and 1.5–350 μM, respectively. At the same time, the proposed method was successfully applied for the determination of guanine and adenine in denatured DNA samples with satisfying results. Moreover, the GS/IL/CS modified electrode exhibited good sensitivity, long-term stability and reproducibility for the determination of guanine and adenine.

  2. Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

    Energy Technology Data Exchange (ETDEWEB)

    Ba Xi; Luo Liqiang [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Ding Yaping, E-mail: wdingyp@sina.com [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Zhang Zhen [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Chu Yuliang [Instrumental Analysis and Research Center, Shanghai University, Shanghai 200444 (China); Wang Bijun; Ouyang Xiaoqian [Department of Chemistry, Shanghai University, Shanghai 200444 (China)

    2012-11-08

    Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 {mu}M G, 50.0 {mu}M A, 100.0 {mu}M T and 100.0 {mu}M C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: Black-Right-Pointing-Pointer The sensor exhibited well-separated peaks and low detection limit. Black-Right-Pointing-Pointer The sensor possesses high sensitivity and wide linear range. Black-Right-Pointing-Pointer The sensor was used for simultaneous detection of G, A, T and C successfully. Black-Right-Pointing-Pointer The sensor was applied in a fish sperm DNA sample with satisfactory results. Black-Right-Pointing-Pointer The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

  3. Simultaneous determination of sulphoraphane and sulphoraphane nitrile in Brassica vegetables using ultra-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Alvarez-Jubete, Laura; Smyth, Thomas J; Valverde, Juan; Rai, Dilip K; Barry-Ryan, Catherine

    2014-01-01

    Several analytical methods exist for the determination of sulphoraphane or sulphoraphane nitrile from biological matrices and plant extracts. However, no UPLC-MS/MS method exists for the simultaneous detection of both. To develop and validate an UPLC-MS/MS method for the simultaneous analysis of sulphoraphane and sulphoraphane nitrile from Brassica oleracea L. ssp. italica This method was developed utilising an Acquity BEH C8 column with gradient elution combined with tandem mass spectrometry, using positive electrospray ionisation in multiple reaction monitoring mode. The retention times for sulphoraphane and sulphoraphane nitrile were 0.4 and 0.6 min respectively, and total run time was 3 min. The method was validated for linearity, sensitivity, precision, accuracy, matrix effects and recovery. The method was employed to determine glucoraphanin hydrolysis products in broccoli and the predominant product was found to vary depending on the variety tested. It was also applied to the accurate determination of sulphoraphane and sulphoraphane nitrile in broccoli samples hydrolysed under different conditions. It was observed that the formation of sulphoraphane and sulphoraphane nitrile was influenced by the temperature of the reaction. The validated UPLC-MS/MS method for simultaneous detection of sulphoraphane and sulphoraphane nitrile was shown to be applicable to broccoli plants and is expected to be applicable to other cruciferous sources. Copyright © 2013 John Wiley & Sons, Ltd.

  4. Simultaneous voltammetric determination of tramadol and acetaminophen using carbon nanoparticles modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Ghorbani-Bidkorbeh, Fatemeh; Shahrokhian, Saeed; Mohammadi, Ali; Dinarvand, Rassoul

    2010-01-01

    A sensitive and selective electrochemical sensor was fabricated via the drop-casting of carbon nanoparticles (CNPs) suspension onto a glassy carbon electrode (GCE). The application of this sensor was investigated in simultaneous determination of acetaminophen (ACE) and tramadol (TRA) drugs in pharmaceutical dosage form and ACE determination in human plasma. In order to study the electrochemical behaviors of the drugs, cyclic and differential pulse voltammetric studies of ACE and TRA were carried out at the surfaces of the modified GCE (MGCE) and the bare GCE. The dependence of peak currents and potentials on pH, concentration and the potential scan rate were investigated for these compounds at the surface of MGCE. Atomic force microscopy (AFM) was used for the characterization of the film modifier and its morphology on the surface of GCE. The results of the electrochemical investigations showed that CNPs, via a thin layer model based on the diffusion within a porous layer, enhanced the electroactive surface area and caused a remarkable increase in the peak currents. The thin layer of the modifier showed a catalytic effect and accelerated the rate of the electron transfer process. Application of the MGCE resulted in a sensitivity enhancement and a considerable decrease in the anodic overpotential, leading to negative shifts in peak potentials. An optimum electrochemical response was obtained for the sensor in the buffered solution of pH 7.0 and using 2 μL CNPs suspension cast on the surface of GCE. Using differential pulse voltammetry, the prepared sensor showed good sensitivity and selectivity for the determination of ACE and TRA in wide linear ranges of 0.1-100 and 10-1000 μM, respectively. The resulted detection limits for ACE and TRA was 0.05 and 1 μM, respectively. The CNPs modified GCE was successfully applied for ACE and TRA determinations in pharmaceutical dosage forms and also for the determination of ACE in human plasma.

  5. A novel UHPLC method for the rapid and simultaneous determination of daidzein, genistein and equol in human urine.

    Science.gov (United States)

    Redruello, Begoña; Guadamuro, Lucía; Cuesta, Isabel; Álvarez-Buylla, Jorge R; Mayo, Baltasar; Delgado, Susana

    2015-11-15

    This work reports on a novel method involving reverse-phased ultra-high performance liquid chromatography (UHPLC) plus a spectrophotometric photodiode array/fluorescence (FLR) detection system for determining the concentration of equol and major soy isoflavones (daidzein and genistein) in human urine. The proposed method was validated in terms of its linearity, sensitivity, accuracy (recovery) and precision (intra- and inter-day repeatability). The isoflavone profiles of urine samples from a group of menopausal women following oral soy isoflavone supplementation were determined and compared. Screening for equol-producer status was accomplished with high sensitivity (detection limit of the FLR detector 2.93nM). The method involves a short chromatographic run time compared to conventional HPLC methods while allowing for the simultaneous and reliable quantification of daidzein, genistein and equol in human urine. It also allows for the rapid screening of multiple urine samples when testing for equol production status and checking patient adherence to isoflavone treatment regimens. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Simultaneous determination of rifabutin and human serum albumin in pharmaceutical formulations by capillary electrophoresis.

    Science.gov (United States)

    Ermolenko, Yu; Anshakova, A; Osipova, N; Kamentsev, M; Maksimenko, O; Balabanyan, V; Gelperina, S

    Capillary zone electrophoresis (CZE) was used for determination of rifabutin (RFB), an anti-tuberculosis antibiotic drug, in various pharmaceutical formulations. Apart from that, simultaneous determination of RFB and human serum albumin (HSA) was performed. Electrophoretic behaviour of RFB was examined at various pH levels. CE conditions: a quartz capillary tube (internal diameter 75mm, effective length 50cm, total length 60cm), the capillary temperature was 25°С, the voltage applied to the capillary tube was +20kV, the UV detection wavelength was 214nm, hydrodynamic injection of the sample was performed at 30mbar for 5s, tetraborate buffer solution (0.01М, рН9.2). The obtained results are characterized by high efficiency (number of theoretical plates up to 260,000) and sufficient sensitivity (LOQ starting from 0.02μg/ml for RFB). The obtained data are in good accord with both HPLC results (for RFB) and spectrophotometry (for HSA). Copyright © 2017 Elsevier Inc. All rights reserved.

  7. Simultaneous Determination of Metals in Coal with Low-Resolution ...

    African Journals Online (AJOL)

    The setup including low-resolution spectrometer with the charge-coupled device (CCD) detector, continuum radiation source and filter furnace (FF) atomizer was employed for direct simultaneous determination of Al, Fe, Mg, Cu and Mn in coal slurry. In the FF, sample vapour entered absorption volume by filtering through ...

  8. Graphitic carbon nitride nanosheets doped graphene oxide for electrochemical simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Zhang, Hanqiang; Huang, Qitong; Huang, Yihong; Li, Feiming; Zhang, Wuxiang; Wei, Chan; Chen, Jianhua; Dai, Pingwang; Huang, Lizhang; Huang, Zhouyi; Kang, Lianping; Hu, Shirong; Hao, Aiyou

    2014-01-01

    Graphical abstract: Schematic drawing of electrochemical oxidize AA, DA and UA on graphitic carbon nitride nanosheets-graphene oxide composite modified electrode. - Highlights: • Synthesize g-C 3 N 4 , GO and CNNS-GO composite. • CNNS-GO composite was the first time for simultaneous determination of AA, DA and UA. • CNNS-GO/GCE displays fantastic selectivity and sensitivity for AA, DA and UA. • CNNS-GO/GCE was applied to detect real sample with satisfactory results. - Abstract: Graphitic carbon nitride nanosheets with a graphite-like structure have strong covalent bonds between carbon and nitride atoms, and nitrogen atoms in the carbon architecture can accelerate the electron transfer and enhance electrical properties effectually. The graphitic carbon nitride nanosheets-graphene oxide composite was synthesized. And the electrochemical performance of the composite was investigated by cyclic voltammetry and differential pulse voltammetry ulteriorly. Due to the synergistic effects of layer-by-layer structures by π-π stacking or charge-transfer interactions, graphitic carbon nitride nanosheets-graphene oxide composite can improved conductivity, electro-catalytic and selective oxidation performance. The proposed graphitic carbon nitride nanosheets-graphene oxide composite modified electrode was employed for simultaneous determination of ascorbic acid, dopamine and uric acid in their mixture solution, it exhibited distinguished sensitivity, wide linear range and low detection limit. Moreover, the modified electrode was applied to detect urine and dopamine injection sample, and then the samples were spiked with certain concentration of three substances with satisfactory recovery results

  9. Simultaneous HPTLC determination of strychnine and brucine in strychnos nux-vomica seed

    Directory of Open Access Journals (Sweden)

    Abid Kamal

    2012-01-01

    Full Text Available Objective: A simple, sensitive, and specific thin layer chromatography (TLC densitometry method has been developed for the simultaneous quantification of strychnine and brucine in the seeds of Strychnos nux-vomica. Materials and Methods: The method involved simultaneous estimation of strychnine and brucine after resolving it by high performance TLC (HPTLC on silica gel plate with chloroform-methanol-formic acid (8.5:1.5:0.4 v/v/v as the mobile phase. Results: The method was validated as per the ICH guidelines for precision (interday, intraday, intersystem, robustness, accuracy, limit of detection, and limit of quantitation. The relationship between the concentration of standard solutions and the peak response was linear within the concentration range of 50-1000 ng/spot for strychnine and 100-1000 ng/spot for brucine. The method precision was found to be 0.58-2.47 (% relative standard deviation [RSD] and 0.36-2.22 (% RSD for strychnine and brucine, respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.75% for strychnine and 100.52% for brucine, respectively. Conclusions: The HPTLC method for the simultaneous quantification of strychnine and brucine was found to be simple, precise, specific, sensitive, and accurate and can be used for routine analysis and quality control of raw material of S. nux-vomica and several unani and ayurvedic formulations containing this as an ingredient.

  10. Cascaded-cavity Fabry-Perot interferometer for simultaneous measurement of temperature and strain with cross-sensitivity compensation

    Science.gov (United States)

    Tian, Jiajun; Jiao, Yuzhu; Ji, Shaobo; Dong, Xiaolong; Yao, Yong

    2018-04-01

    We propose and demonstrate a fiber sensor for simultaneous temperature and strain measurements. The proposed sensor is implemented by a cascaded-cavity Fabry-Perot (FP) fiber interferometer. The two cascaded FP cavities comprise a micro-air-cavity in a hollow-core tube fiber and a micro-silica-cavity in a standard single-mode fiber. To separate the interference spectrum of each FP cavity, the total spectrum is filtered in the frequency domain through band-pass filters, whose central frequencies were predesigned based on the relationship between the spatial frequency and free spectral range of each FP cavity. The different cross-sectional areas and thermal-optic coefficients of the two FP cavities confer different sensitivities to temperature and strain. Both parameters were measured simultaneously by tracking the wavelength shifts in the filtered interference spectra of the FP cavities. Moreover, the temperature-strain cross-sensitivity was compensated by solving a sensitivity-coefficient matrix equation for the two cavities, using the calibrated temperatures and strains. Other advantages of the proposed sensor are simple fabrication and an all-fiber structure. Owing to these properties, the proposed sensor is potentially applicable to real sensing applications.

  11. Simultaneous acquisition of X-ray spectra using a multi-wire, position-sensitive gas flow detector

    International Nuclear Information System (INIS)

    Beaven, Peter A.; Marmotti, Mauro; Kampmann, Reinhard; Knoth, Joachim; Schwenke, Heinrich

    2003-01-01

    A multi-wire, gas-filled position-sensitive detector has been developed for the simultaneous recording of wavelength-dispersed X-ray signals that enables X-ray fluorescence spectrometry with a limited multi-element capability in the low Z element range. Details of the modular construction of the detector are given. The detector performance was characterized using Al-Kα radiation and a variable slit system. The detector has been applied in a laboratory spectrometer equipped with an electron source and a double multilayer mirror device as the wavelength-dispersing element. Spectra from Al and Si obtained in the simultaneous acquisition mode show good agreement with calculations performed using a ray-tracing model

  12. Improvement on simultaneous determination of chromium species in aqueous solution by ion chromatography and chemiluminescence detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Liao, Y.P.; Jons, O.

    1997-01-01

    A sensitive method for the simultaneous determination of chromium(III) and chromium(VI) was chromatography and chemiluminescence detection. Two Dionex ion-exchange guard columns in series, CG5 and AG7, were used to separate chromium(III) from chromium(VI). Chromium(VI) was reduced by potassium......, the stabilities of reductant and luminol solutions were studied. The linear range of the calibration curve for chromium(III) and chromium(VI) was 1-400 mu g l(-1). The detection limit was 0.12 mu g l(-1) for chromium(III) and 0.09 mu g l(-1) for chromium(VI), respectively. The precision at the 20 mu g l(-1) level...... was 1.4% for chromium(III) and 2.5% for chromium(VI), respectively. The accuracy of the chromium(III) determination was determined by analysis of the NIST standard reference material 1643c, Trace elements in water with the result 19.1 +/- 1.0 mu g Cr(III) l(-1) (certified value 19.0 +/- 0.6 mu g Cr...

  13. Enzymatic biosensor of horseradish peroxidase immobilized on Au-Pt nanotube/Au-graphene for the simultaneous determination of antioxidants

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Long; Yin, Wenmin; Tang, Kun; Li, Dian; Shao, Kang; Zuo, Yunpeng; Ma, Jing; Liu, Jiawei; Han, Heyou, E-mail: hyhan@mail.hzau.edu.cn

    2016-08-24

    A new electrochemical method has been proposed for the simultaneous determination of butylated hydroxyanisole (BHA) and propyl gallate (PG) in food matrices based on enzymatic biosensors. Spiny Au-Pt nanotubes (SAP NTs) was first synthesized and demonstrated to exhibit intrinsic peroxidase and catalase-like activity. The structure of SAP NTs provides large surface area and favorable medium for electron transfer, on which HRP were immobilized and acted as enzymatic biosensor for the simultaneous detection of BHA and PG. The results revealed that BHA and PG both have well-defined oxidation waves with peak potentials of 624 and 655 mV, respectively. Under the optimal conditions, the method behaved satisfactory analytical performance towards BHA and PG with a wide linear range of 0.3–50 mg L{sup −1} and 0.1–100 mg L{sup −1}, as well as a detection limit of 0.046 mg L{sup −1} and 0.024 mg L{sup −1} (3σ/slope), respectively. Besides, the proposed method exhibits good sensitivity, stability and reproducibility, providing an alternative to fabricate electrode and construct sensitive biosensors. - Highlights: • SAP NTs was synthesized and demonstrated to exhibit intrinsic peroxidase and catalase-like activity. • The structure of SAP NTs provides larger surface area and more favorable medium for electron transfer. • Horseradish peroxidase immobilized on Au-Pt nanotube/Au-graphene acted as enzymatic biosensor. • The simultaneous detection of BHA and PG in food matrices was achieved based on enzymatic biosensors.

  14. Simultaneous kinetic spectrometric determination of three flavonoid antioxidants in fruit with the aid of chemometrics

    Science.gov (United States)

    Sun, Ruiling; Wang, Yong; Ni, Yongnian; Kokot, Serge

    2014-03-01

    A simple, inexpensive and sensitive kinetic spectrophotometric method was developed for the simultaneous determination of three anti-carcinogenic flavonoids: catechin, quercetin and naringenin, in fruit samples. A yellow chelate product was produced in the presence neocuproine and Cu(I) - a reduction product of the reaction between the flavonoids with Cu(II), and this enabled the quantitative measurements with UV-vis spectrophotometry. The overlapping spectra obtained, were resolved with chemometrics calibration models, and the best performing method was the fast independent component analysis (fast-ICA/PCR (Principal component regression)); the limits of detection were 0.075, 0.057 and 0.063 mg L-1 for catechin, quercetin and naringenin, respectively. The novel method was found to outperform significantly the common HPLC procedure.

  15. Simultaneous determination of uranium and thorium with Arsenazo III by second-derivative spectrophotometry

    International Nuclear Information System (INIS)

    Kuroda, Rokuro; Kurosaki, Mayumi; Hayashibe, Yutaka; Ishimaru, Satomi

    1990-01-01

    A derivative spectrophotometric method has been developed for the simultaneous determination of microgram quantities of uranium and thorium with Arsenazo III in hydrochloric acid medium. The second-derivative absorbances of the uranium and thorium Arsenazo III complexes at 679.5 and 684.4 nm are used for their quantification. Uranium and thorium, both in the range 0.1-0.7 μg/ml have been determined simultaneously with good precision. The procedure does not require separation of uranium and thorium, and allows the determination of both metals in the presence of alkaline-earth metals and zirconium, but lanthanides interfere. (author)

  16. H-point standard additions method for simultaneous determination of sulfamethoxazole and trimethoprim in pharmaceutical formulations and biological fluids with simultaneous addition of two analytes

    Science.gov (United States)

    Givianrad, M. H.; Saber-Tehrani, M.; Aberoomand-Azar, P.; Mohagheghian, M.

    2011-03-01

    The applicability of H-point standard additions method (HPSAM) to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim is verified by UV-vis spectrophotometry. The results show that the H-point standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. The results of applying the H-point standard additions method showed that the two drugs could be determined simultaneously with the concentration ratios of sulfamethoxazole to trimethoprim varying from 1:18 to 16:1 in the mixed samples. Also, the limits of detections were 0.58 and 0.37 μmol L -1 for sulfamethoxazole and trimethoprim, respectively. In addition the means of the calculated RSD (%) were 1.63 and 2.01 for SMX and TMP, respectively in synthetic mixtures. The proposed method has been successfully applied to the simultaneous determination of sulfamethoxazole and trimethoprim in some synthetic, pharmaceutical formulation and biological fluid samples.

  17. Sensitive and simultaneous quantification of zinc pyrithione and climbazole deposition from anti-dandruff shampoos onto human scalp

    NARCIS (Netherlands)

    Chen, G.; Miao, M.; Hoptroff, M.; Fei, X.; Collins, L.Z.; Jones, A.; Janssen, H.G.

    2015-01-01

    A sensitive ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method has been developed and validated for simultaneous quantification of zinc pyrithione (ZPT) and climbazole (CBZ) deposited onto human scalp from anti-dandruff (AD) shampoos. Scrubbing with a buffer

  18. Simultaneous determination of non-steroidal anti-inflammatory drugs in pharmaceutical formulations and human serum by reversed phase high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Muhammad Nawaz

    2012-01-01

    Full Text Available A rapid and sensitive method using high performance liquid chromatography has been developed and validated for the simultaneous determination of non-steroidal anti-inflammatory drugs (NSAIDs in pharmaceutical formulations and human serum. Six NSAIDs including: naproxen sodium, diclofenac sodium, meloxicam, flurbiprofen, tiaprofenic and mefenamic acid were analyzed simultaneously in presence of ibuprofen as internal standard on Mediterranea C18 (5 µm, 250 x 0.46 mm column. Mobile phase comprised of methanol: acetonitrile: H2O (60:20:20, v/v; pH 3.35 and pumped at a flow rate of 1 mL min-1 using 265 nm UV detection. The method was linear over a concentration range of 0.25-50 µg mL-1 (r² = 0.9999.

  19. Two different spectrofluorimetric methods for simultaneous determination of gemfibrozil and rosiglitazone in human plasma.

    Science.gov (United States)

    El-Din, Mohie M K Sharaf; Attia, Khalid A M; Nassar, Mohamed W I; Kaddah, Mohamed M Y

    2010-10-15

    Two accurate, reliable, and highly sensitive spectrofluorimetric methods were developed for simultaneous determination of binary mixture gemfibrozil and rosiglitazone in human plasma without prior separation steps. The first method is based on synchronous fluorescence spectrometry using double scans. At Δλ=27nm, gemfibrozil yields detectable signal that is independent of the presence of rosiglitazone. Similarly, at Δλ=120nm the signal of rosiglitazone is not influenced by the presence of gemfibrozil. Signals at two wavelengths, 301 (Δλ=27nm) and 368nm (Δλ=120nm) vary linearly with gemfibrozil and rosiglitazone concentrations over the range 100-700ngmL(-1) (for gemfibrozil) and 20-140ngmL(-1) (for rosiglitazone), respectively. The limits of detection (LOD) were 2.3 and 2.72ngmL(-1) for gemfibrozil and rosiglitazone, respectively. The second method is based on the technique of simultaneous equations (Vierodt's method), in which 258nm was selected as the excitation wavelength. Two equations are constructed based on the fact that at ( λ(EM)₂=302 nm of gemfibrozil) and (λ(EM)₂=369 nm of rosiglitazone) the fluorescence of the mixture is the sum of the individual fluorescence of gemfibrozil and rosiglitazone. The limits of detection (LOD) were 28.1 and 23.63ngmL(-1) for gemfibrozil and rosiglitazone, respectively. The proposed methods were successfully applied for the determination of the two compounds in synthetic mixtures and in human plasma with a good recovery. Copyright © 2010 Elsevier B.V. All rights reserved.

  20. Development and validation of an HPLC method for simultaneous determination of trimethoprim and sulfamethoxazole in human plasma.

    Science.gov (United States)

    Sayar, Esin; Sahin, Selma; Cevheroglu, Semsettin; Hincal, A Atilla

    2010-09-01

    The combination of trimethoprim (TMP) and sulfamethoxazole (SMX) is used in the treatment of many common infections such as urinary, respiratory and gastrointestinal tract infections. The aim of this study was to determine TMP and SMX simultaneously in human plasma samples by high performance liquid chromatography (HPLC) using antipyrine as the internal standard. Separation of the compounds was achieved on a reverse-phase C8 column packed with 5 microm dimethyl octadecylsilyl bonded amorphous silica (4.6 mm x 250 mm) column using a mobile phase consisted of potassium hydrogen phosphate, acetonitrile, methanol and water adjusted to pH 6.2. The mobile phase was delivered at a flow rate of 1 mL min- and the effluent was monitored using Max plot technique at 25 derees C. Retention times were 5 min for TMP, 7 min for antipyrine and 9 min for SMX. Quantitation limits were 10 ng mL(-1) for TMP and 50 ng mL(-1) for SMX. Our findings indicated that the developed HPLC method was precise, accurate, specific and sensitive for simultaneous determination of TMP and SMX. Proposed HPLC method was successfully applied for the analysis of TMP and SMX in human plasma after oral administration of a co-trimoxazole tablet to human volunteers.

  1. Simultaneous Determination of Co-formulated Matrine and ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a new, simple, sensitive and accurate high performance liquid chromatographic (HPLC) method for the simulataneous determination of matrine and secnidazole in suppositories. Methods: The method involved using a SinoChoom ODS-BP C18 column (5 ƒÊm, 4.6 mm ~ 200 mm) and ...

  2. [An ultrafast liquid chromatography-tandem mass spectrometric method for simultaneous determination of common artificial synthetic pigments in cooked meat products].

    Science.gov (United States)

    Chen, Xiaohong; Li, Xiaoping; Zhao, Yonggang; Pan, Shengdong; Jin, Micong

    2015-07-01

    A method based on ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) has been developed for the simultaneous determination of seven synthetic pigments in cooked meat product. After the cooked meat products were extracted by mixed extraction agent, purified by WAX column, the UFLC separation was performed on a Shim-pack XR-ODS II column (75 mm x 2.0 mm, 2.2 µm) with a linear gradient elution program of acetonitrile and ammonium acetate (AmAc, 5 mmol/L) as the mobile phase. Electrospray ionization was applied and operated in the negative ion mode. The limits of quantitation (LOQs) for the seven synthetic pigments were in the range of 0.7-5.0 µg/kg. The calibration curves showed good linearities for the seven analytes in their detection ranges, and the correlative coefficients (r) were more than 0.999. The recoveries were between 88.2%-106.5% with the RSDs in the range of 1.2%-5.0%. The method is sensitive, reproducible, quick and adapts to the simultaneous determination of the seven synthetic pigments in cooked meat product.

  3. [Simultaneous determination of eleven components in Ginkgo biloba leaves by high performance liquid chromatography method].

    Science.gov (United States)

    Lv, Jin-Li; Yang, Biao; Li, Meng-Xuan; Meng, Zhao-Qing; Ma, Shi-Ping; Wang, Zhen-Zhong; Ding, Gang; Huang, Wen-Zhe; Xiao, Wei

    2017-03-01

    To study Ginkgo biloba leaves in different producing area, we establish an HPLC method for the simultaneously determination of seven flavonoids glycosides and four biflavonoids in G. biloba leaves. The analysis was performed on an Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm, 5 μm) wich acetonitrile, and 0.4% phosphoric acid as mobile phase at flow rate of 1 mL•min⁻¹ in a gradient edution, and the detection was carried out at 254 nm.The calibration curves of the seven flavonoids glycosides and four biflavonoids had a good linearitiy with good recoveries. The established HPLC method is simple, rapid, accurate, reliable, and sensitive, and can be applied to the identification and quality control of G. biloba leaves. Copyright© by the Chinese Pharmaceutical Association.

  4. MgO nanobelt-modified graphene-tantalum wire electrode for the simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Zhao, Liwei; Li, Hongji; Gao, Sumei; Li, Mingji; Xu, Sheng; Li, Cuiping; Guo, Wenlong; Qu, Changqing; Yang, Baohe

    2015-01-01

    Graphical abstract: Display Omitted -- Highlights: •Graphene and MgO nanobelts are deposited on tantalum wires to form biosensors. •Ascorbic acid, dopamine and uric acid are determined with the biosensors. •The biosensors show high electrocatalytic activity for oxidation of these species. •The biosensors show high selectivity and good sensitivity. -- ABSTRACT: A promising electrochemical biosensor for simultaneous detection of ascorbic acid (AA), dopamine (DA) and uric acid (UA) was fabricated by electrochemical deposition of MgO nanobelts on a graphene-modified tantalum wire (denoted as MgO/Gr/Ta) electrode. The MgO nanobelts and graphene were verified by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Electrochemical performances of the electrodes were characterized by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The CV results show that AA, DA and UA could be detected simultaneously using MgO/Gr/Ta electrode with peak-to-peak separation of 300 mV, 147 mV and 447 mV for AA-DA, DA-UA and AA-UA, respectively. In the threefold co-existence system, the linear calibration plots for AA, DA and UA were obtained over the concentration range of 5.0–350 μM, 0.1–7 μM and 1–70 μM with detection limits of 0.03 μM, 0.15 μM and 0.12 μM, respectively. The modified electrode shows excellent selectivity, good sensitivity and good stability, making it attractive as a sensor for simultaneous detection of AA, DA and UA in biological fluids

  5. Simultaneous determination of amino acid and monoamine neurotransmitters in PC12 cells and rats models of Parkinson's disease using a sensitizing derivatization reagent by UHPLC-MS/MS.

    Science.gov (United States)

    Zhao, Xian-En; Zhu, Shuyun; Yang, Hongmei; You, Jinmao; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

    2015-07-15

    Multi-analytes simultaneous monitoring of amino acid and monoamine neurotransmitters (NTs) has important scientific significance for their related pathology, physiology and drug screening. In this work, in virtue of a mass spectrometry sensitizing reagent 10-ethyl-acridone-3-sulfonyl chloride (EASC) as derivatization reagent, an Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS) method was developed and validated for simultaneous determination of six amino acid NTs, two monoamine ones and its one metabolite. The simple and rapid derivatization reaction was innovatively combined with plasma preparation by using EASC acetonitrile solution as protein precipitant. This interesting combination brought the advantages of speediness, simpleness and high-throughput in a cost-effective way. Under the optimized conditions, LODs (0.004-3.80nM) and LOQs (0.014-13.3nM) of EASC derivatized-NTs were calculated and found to be significantly lower than those of direct UHPLC-MS/MS detection about 11.5-275.0 and 14.4-371.4 times, respectively. Moreover, EASC derivatization significantly improved chromatographic resolution and matrix effect when compared with direct UPLC-MS/MS detection method without derivatization. Meanwhile, it also brought acceptable precision (3.0-13.0%, peak area CVs%), accuracy (86.4-112.9%), recovery (88.3-107.8%) and stability (3.8-8.5%, peak area CVs%) results. This method was successfully applied for the antiparkinsonian effect evaluation of levodopa and Ginsenoside Rg1 using PC12 cells and rats models by measuring multiple NTs. This provided a new method for the NTs related studies in the future. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Simultaneous determination of total arsenic and total selenium in Chinese medicinal herbs by hydride generation atomic fluorescence spectrometry in tartaric acid medium

    International Nuclear Information System (INIS)

    Liu Zhanfeng; Sun Hanwen; Shen Shigang; Li Liqing; Shi Hongmei

    2005-01-01

    By HG-AFS, a new method was proposed for simultaneous determination of total arsenic and total selenium existed in the Chinese medicinal herbs in tartaric acid medium. The effects of analytical conditions and coexisting ions on the fluorescence signal intensity of analytes were investigated. The proposed method was provided with linear response ranges above 22 μg l -1 for As and 44 μg l -1 for Se, and the detection limits of 0.13 and 0.12 μg l -1 were obtained for As and Se respectively. The recoveries of 93.8-96.1% for As and 95.3-99.1% for Se, and the precision of 1.2-3.8% and 2.4-5.3% (R.S.D., n = 8) respectively, were obtained via simultaneous determined four samples of Chinese medicinal herbs and three certified botanic reference materials successfully. The proposed method has the advantages of simple operation, high sensitivity and high efficiency

  7. Simultaneous Determination of Multi-Mycotoxins in Cereal Grains Collected from South Korea by LC/MS/MS

    Directory of Open Access Journals (Sweden)

    Dong-Ho Kim

    2017-03-01

    Full Text Available An improved analytical method compared with conventional ones was developed for simultaneous determination of 13 mycotoxins (deoxynivalenol, nivalenol, 3-acetylnivalenol, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, fumonisin B1, fumonisin B2, T-2, HT-2, zearalenone, and ochratoxin A in cereal grains by liquid chromatography-tandem mass spectrometry (LC/MS/MS after a single immunoaffinity column clean-up. The method showed a good linearity, sensitivity, specificity, and accuracy in mycotoxin determination by LC/MS/MS. The levels of 13 mycotoxins in 5 types of commercial grains (brown rice, maize, millet, sorghum, and mixed cereal from South Korea were determined in a total of 507 cereal grains. Mycotoxins produced from Fusarium sp. (fumonisins, deoxynivalenol, nivalenol, and zearalenone were more frequently (more than 5% and concurrently detected in all cereal grains along with higher mean levels (4.3–161.0 ng/g in positive samples than other toxins such as aflatoxins and ochratoxin A (less than 9% and below 5.2 ng/g in positive samples from other fungal species.

  8. Simultaneous determination of Sunset yellow and Tartrazine in soft drinks using gold nanoparticles carbon paste electrode.

    Science.gov (United States)

    Ghoreishi, Sayed Mehdi; Behpour, Mohsen; Golestaneh, Mahshid

    2012-05-01

    The monitoring of synthetic dyes in foods is very important due to their potential harmfulness to human beings. Herein, a carbon-paste electrode (CPE) that is chemically modified with gold nanoparticles (nAu) was fabricated and used for the determination of Sunset yellow (SY) and Tartrazine (Tz). Cyclic and differential pulse voltammetry (CV and DPV) results revealed two well-resolved anodic peaks for SY and Tz with remarkably increase in oxidation signals of these colourants. Based on this, a novel electrochemical method was developed for the simultaneous determination of SY and Tz. High sensitivity and selectivity, sub-micromolar detection limit, high reproducibility and regeneration of the electrode surface by simple polishing make the nAu-CPE electrode very suitable for the determination of SY and Tz in commercially available soft drinks. The detection limits was 3.0×10(-8) and 2.0×10(-9)moll(-1) for SY and Tz, respectively, which are remarkably lower than those reported previously for SY and Tz using other modified electrodes. Copyright © 2011 Elsevier Ltd. All rights reserved.

  9. Simultaneous determination of environmental α-radionuclides using liquid scintillation counting combined with time interval analysis (TIA) and pulse shape discrimination (PSD)

    International Nuclear Information System (INIS)

    Hashimoto, T.; Sato, K.; Yoneyama, Y.; Fukuyama, N.

    1997-01-01

    Some improvements of the detection sensitivity in pulse time interval analysis (TIA) based on selective extraction of successively α-α correlated decay events within millisecond order from random or background events, were established by the utilization of PSD, to reject β/γ-pulses from α-ones and a simple chemical procedure of radium separation, together with the use of well resolved scintillator. By applying the PSD, the contribution of β-decay events was completely eliminated in both the α-spectra and the TIA distribution curves as well as the improvement into clear energy resolution and the enhancement of detection sensitivity for the TIA. As a result, the TIA and α-spectrometric analysis of 226 Ra-extract showed the existence of 223 Ra (Ac-series) and β/α-correlated events with correlated life (due to 0.16 ms due to 214 Bi(β)-> 214 Po(α)->) along with a singly well resolved α-peak to be useful for the determination of 226 Ra (U-series). The difference of half-lives (145 and 1.78 ms) due to 216 Po and 215 Po (direct daughters of 224 Ra for Th-series and 223 Ra for Ac-series, respectively) was also proven for the possibility of the simultaneous determination of both correlated events by using the TIA/PSD combined with chemical separation and liquid scintillation counting method. Finally, the simultaneous determination of three natural decay series, which include U-, Th- and Ac-series nuclides, have been conveniently carried out for some environmental samples using the present method combined with 225 Ra yield tracer (Np-series). (author)

  10. Simultaneous Determination of Tizanidine, Nimesulide, Aceclofenac and Paracetamol in Tablets and Biological Fluids Using Micellar Liquid Chromatography.

    Science.gov (United States)

    Belal, Fathalla; Omar, Mahmoud A; Derayea, Sayed; Hammad, Mohamed A; Zayed, Sahar; Saleh, Safaa F

    2018-03-01

    A simple, sensitive and rapid micellar liquid chromatographic method was developed and validated for simultaneous determination of four drugs, namely, paracetamol (PAR), tizanidine (TZD), aceclofenac (ACF) and nimesulide (NMD). Good chromatographic separation was achieved using Cyano column and micellar mobile phase consisting of 120 mM sodium dodecyl sulfate, 25 mM phosphate buffer and 10% (V/V) butanol. The pH was adjusted to three using phosphoric acid. The total retention time was below 10 min. The analysis was performed at a flow rate of 1 mL/min and a column temperature of 40°C with direct UV detection at 230 nm. Diclofenac sodium was used as the internal standard. The proposed method was validated according to the ICH guidelines and was successfully applied to the analysis of these drugs in their tablet dosage forms with high accuracy. Limits of detection were found to be 0.03, 0.07, 0.033 and 0.11 μg/mL for PAR, ACF, TZD and NMD, respectively. The high sensitivity of developed method permitted its application to the in-vitro determination of the cited drugs in spiked human plasma and urine samples, and the obtained results were satisfactory. However, PAR could not be determined in spiked human urine because its peak overlapped with that of the urine peak.

  11. Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

    Science.gov (United States)

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

  12. Simultaneous determination of left ventricular perfusion and function

    International Nuclear Information System (INIS)

    Gremillet, E.; Champailler, A.; Esquerre, J.P.; Ouhayoun, E.; Coca, F.; Furber, A.; Le Jeune, J.J.

    1997-01-01

    Myocardial perfusion scintigraphy is a very useful tool for the diagnosis and prognosis of coronary artery disease. The evaluation of left ventricular function during stress testing in also very useful to determine the prognosis of coronary artery disease. This chapter highlights three different imaging methods to assess left ventricular function and myocardial perfusion/ The first one consists of sequential dual isotope myocardial SPECT with ECG-gating. The second concerns magnetic resonance imaging and the third explores first pass exercise ventriculography and myocardial perfusion scintigraphy simultaneously evaluated by means of 99m Tc-sestamibi. (authors)

  13. Simultaneous determination of nikethamide and lidocaine in human blood and cerebrospinal fluid by high performance liquid chromatography.

    Science.gov (United States)

    Chen, Lili; Liao, Linchuan; Zuo, Zhong; Yan, Youyi; Yang, Lin; Fu, Qiang; Chen, Yu; Hou, Junhong

    2007-04-11

    Nikethamide and lidocaine are often requested to be quantified simultaneously in forensic toxicological analysis. A simple reversed-phase high performance liquid chromatography (RP-HPLC) method has been developed for their simultaneous determination in human blood and cerebrospinal fluid. The method involves simple protein precipitation sample treatment followed by quantification of analytes using HPLC at 263 nm. Analytes were separated on a 5 microm Zorbax Dikema C18 column (150 mm x 4.60 mm, i.d.) with a mobile phase of 22:78 (v/v) mixture of methanol and a diethylamine-acetic acid buffer, pH 4.0. The mean recoveries were between 69.8 and 94.4% for nikethamide and between 78.9 and 97.2% for lidocaine. Limits of detection (LODs) for nikethamide and lidocaine were 0.008 and 0.16 microg/ml in plasma and 0.007 and 0.14 microg/ml in cerebrospinal fluid, respectively. The mean intra-assay and inter-assay coefficients of variation (CVs) for both analytes were less than 9.2 and 10.8%, respectively. The developed method was applied to blood sample analyses in eight forensic cases, where blood concentrations of lidocaine ranged from 0.68 to 34.4 microg/ml and nikethamide ranged from 1.25 to 106.8 microg/ml. In six cases cerebrospinal fluid analysis was requested. The values ranged from 20.3 to 185.6 microg/ml of lidocaine and 8.0 to 72.4 microg/ml of nikethamide. The method is simple and sensitive enough to be used in toxicological analysis for simultaneous determination of nikethamide and lidocaine in blood and cerebrospinal fluid.

  14. Development and validation of a rapid, selective, and sensitive LC-MS/MS method for simultaneous determination of D- and L-amino acids in human serum: application to the study of hepatocellular carcinoma.

    Science.gov (United States)

    Han, Minlu; Xie, Mengyu; Han, Jun; Yuan, Daoyi; Yang, Tian; Xie, Ying

    2018-04-01

    A validated liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of D- and L-amino acids in human serum. Under the optimum conditions, except for DL-proline, L-glutamine, and D-lysine, the enantioseparation of the other 19 enantiomeric pairs of proteinogenic amino acids and nonchiral glycine was achieved with a CROWNPAK CR-I(+) chiral column within 13 min. The lower limits of quantitation for L-amino acids (including glycine) and D-amino acids were 5-56.25 μM and 0.625-500 nM, respectively, in human serum. The intraday precision and interday precision for all the analytes were less than 15%, and the accuracy ranged from -12.84% to 12.37% at three quality control levels. The proposed method, exhibiting high rapidity, enantioresolution, and sensitivity, was successfully applied to the quantification of D- and L-amino acid levels in serum from hepatocellular carcinoma patients and healthy individuals. The serum concentrations of L-arginine, L-isoleucine, L-aspartate, L-tryptophan, L-alanine, L-methionine, L-serine, glycine, L-valine, L-leucine, L-phenylalanine, L-threonine, D-isoleucine, D-alanine, D-glutamate, D-glutamine, D-methionine, and D-threonine were significantly reduced in the hepatocellular carcinoma patients compared with the healthy individuals (P hepatocellular carcinoma research. Graphical abstract Simultaneous determination of D- and L-amino acids in human serum from hepatocellular carcinoma patients and healthy individuals. AA amino acid, HCC hepatocellular carcinoma, LC liquid chromatography, MS/MS tandem mass spectrometry, NC normal control, TIC total ion chromatogram.

  15. A highly sensitive electrochemical sensor for simultaneous determination of hydroquinone and bisphenol A based on the ultrafine Pd nanoparticle@TiO2 functionalized SiC

    International Nuclear Information System (INIS)

    Yang, Long; Zhao, Hui; Fan, Shuangmei; Li, Bingchan; Li, Can-Peng

    2014-01-01

    Graphical abstract: The illustration of Pd@TiO 2 –SiC nanohybrids simultaneous sensing hydroquinone and bisphenol A by an electrochemical strategy. - Highlights: • TiO 2 –SiC was successfully prepared by a facile generic in situ growth strategy. • Ultrafine Pd NPs with a uniform size of ∼2.3 nm monodispersed on TiO 2 –SiC surface. • Electrochemical simultaneous determination of HQ and BPA was established. • Ultrafine metal NPs@metal oxide–SiC may be extended to other applications. - Abstract: A titanium dioxide–silicon carbide nanohybrid (TiO 2 –SiC) with enhanced electrochemical performance was successfully prepared through a facile generic in situ growth strategy. Monodispersed ultrafine palladium nanoparticles (Pd NPs) with a uniform size of ∼2.3 nm were successfully obtained on the TiO 2 –SiC surface via a chemical reduction method. The Pd-loaded TiO 2 –SiC nanohybrid (Pd@TiO 2 –SiC) was characterized by transmission electron microscopy and X-ray diffractometry. A method for the simultaneous electrochemical determination of hydroquinone (HQ) and bisphenol A (BPA) using a Pd@TiO 2 –SiC nanocomposite-modified glassy carbon electrode was established. Utilizing the favorable properties of Pd NPs, the Pd@TiO 2 –SiC nanohybrid-modified glassy carbon electrode exhibited electrochemical performance superior to those of TiO 2 –SiC and SiC. Differential pulse voltammetry was successfully used to simultaneously quantify HQ and BPA within the concentration range of 0.01–200 μM under optimal conditions. The detection limits (S/N = 3) of the Pd@TiO 2 –SiC nanohybrid electrode for HQ and BPA were 5.5 and 4.3 nM, respectively. The selectivity of the electrochemical sensor was improved by introducing 10% ethanol to the buffer medium. The practical application of the modified electrode was demonstrated by the simultaneous detection of HQ and BPA in tap water and wastewater samples. The simple and straightforward strategy presented in this

  16. Simultaneous determination of three herbicides by differential pulse voltammetry and chemometrics.

    Science.gov (United States)

    Ni, Yongnian; Wang, Lin; Kokot, Serge

    2011-01-01

    A novel differential pulse voltammetry method (DPV) was researched and developed for the simultaneous determination of Pendimethalin, Dinoseb and sodium 5-nitroguaiacolate (5NG) with the aid of chemometrics. The voltammograms of these three compounds overlapped significantly, and to facilitate the simultaneous determination of the three analytes, chemometrics methods were applied. These included classical least squares (CLS), principal component regression (PCR), partial least squares (PLS) and radial basis function-artificial neural networks (RBF-ANN). A separately prepared verification data set was used to confirm the calibrations, which were built from the original and first derivative data matrices of the voltammograms. On the basis relative prediction errors and recoveries of the analytes, the RBF-ANN and the DPLS (D - first derivative spectra) models performed best and are particularly recommended for application. The DPLS calibration model was applied satisfactorily for the prediction of the three analytes from market vegetables and lake water samples.

  17. Simultaneous bulk density and soil moisture determination by attenuation of 137 Cs and 241 Am

    International Nuclear Information System (INIS)

    Barros Ferraz, E.S. de.

    1974-01-01

    The method of simultaneous bulk density and soil moisture determination by attenuation of 241 Am and 137 Cs gamma-radiation is introduced and studied with detail. Theoretical considerations are made about the attenuation process in the absorbers, the form of solving the problem of two unknowns, the sensitivity of the method the influences of the resolution time of the electronic counting equipment, and of the Compton scattering in the sample. From the methodological point of view studies are made about the influence of the geometry, adjustment of counting system, choice of radiation sources, attenuation coefficient and the manner of obtaining reliable measurements. Data obtained are analysed, discussed and compared with those found in the literature. Finally the author presents some applications of the method, its use in soil-water movement studies, in soil profile compaction studies, and specially in swelling soils. (author)

  18. Simultaneous LC-MS/MS determination of phenylbutyrate, phenylacetate benzoate and their corresponding metabolites phenylacetylglutamine and hippurate in blood and urine.

    Science.gov (United States)

    Laryea, Maurice D; Herebian, Diran; Meissner, Thomas; Mayatepek, Ertan

    2010-12-01

    Inborn errors of urea metabolism result in hyperammonemia. Treatment of urea cycle disorders can effectively lower plasma ammonium levels and results in survival in the majority of patients. Available medications for treating urea cycle disorders include sodium benzoate (BA), sodium phenylacetate (PAA), and sodium phenylbutyrate (PBA) and are given to provide alternate routes for disposition of waste nitrogen excretion. In this study, we develop and validate a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of benzoic acid, phenylacetic acid, phenylbutyric acid, phenylacetylglutamine, and hippuric acid in plasma and urine from children with inborn errors of urea synthesis. Plasma extracts and diluted urine samples were injected on a reverse-phase column and identified and quantified by selected reaction monitoring (SRM) in negative ion mode. Deuterated analogues served as internal standards. Analysis time was 7 min. Assay precision, accuracy, and linearity and sample stability were determined using enriched samples. Quantification limits of the method were 100 ng/ml (0.3-0.8 μmol/L) for all analytes, and recoveries were >90%. Inter- and intraday relative standard deviations were <10%. Our newly developed LC-MS/MS represents a robust, sensitive, and rapid method that allows simultaneous determination of the five compounds in plasma and urine.

  19. A new sensor based on glassy carbon electrode modified with nanocomposite for simultaneous determination of acetaminophen, ascorbic acid and uric acid

    Directory of Open Access Journals (Sweden)

    Mohammad Afrasiabi

    2016-09-01

    Full Text Available A chemically-modified electrode has been constructed based on a single walled carbon nanotube/chitosan/room temperature ionic liquid nanocomposite modified glassy carbon electrode (SWCNTs–CHIT–RTIL/GCE. It was demonstrated that this sensor could be used for simultaneous determination of acetaminophen (ACT, uric acid (URI and ascorbic acid (ASC. The measurements were carried out by application of differential pulse voltammetry (DPV, cyclic voltammetry (CV and chronoamperometry (CA methods. Electrochemical studies suggested that the RTIL and SWCNTs provided a synergistic augmentation that can increase current responses by improvement of electron transfers of these compounds on the electrode surface. The presence of the CHIT in the modified electrode can enhance the repeatability of the sensor by its antifouling effect. The modified electrode showed electrochemical responses with high sensitivity for ACT, URI and ASC determination, which makes it a suitable sensor for simultaneous sub-μmol L−1 detection of ACT, URI and ASC in aqueous solutions. The analytical performance of this sensor has been evaluated for detection of ACT, URI and ASC in human serum and urine with satisfactory results.

  20. Electrocatalytic properties of functionalized carbon nanotubes with titanium dioxide and benzofuran derivative/ionic liquid for simultaneous determination of isoproterenol and serotonin

    International Nuclear Information System (INIS)

    Mazloum-Ardakani, Mohammad; Khoshroo, Alireza

    2014-01-01

    Highlights: • TiO 2 and benzofuran derivative were uniformly deposited onto carbon nanotubes • This nanocomposite can be used as a sensor in isoproterenol detection • This sensor shows a great enhancement in sensitivity, selectivity and stability - Abstract: In this paper we report synthesis and application of functionalized multiwalled carbon nanotubes (CNTs) with titanium dioxide nanoparticles (TiO 2 ), 9-(1,3-dithiolan-2-yl)-6,7-dihydroxy-3,3-dimethyl-3,4-dihydrodibenzo[b,d] furan-1(2H)-one (benzofuran derivative (DDF)) and 1-butyl-3-methylimidazolium tetrafluoroborate (IL) as high sensitive sensors for simultaneous determination of isoproterenol (IP) and serotonin (5-HT) using glassy carbon electrode. The modified electrode was characterized by different methods including a scanning electron microscope (SEM), electrochemical impedance spectroscopy (EIS) and voltammetry. A pair of well-defined redox peaks of DDF was obtained at the modified glassy carbon electrode by direct electron transfer between the DDF and the electrode. Dramatically enhanced electrocatalytic activity was exemplified at the modified electrode, as an electrochemical sensor to study the electro oxidation of IP and 5-HT. The differential pulse voltammetry data showed that the obtained anodic peak currents were linearly dependent on the IP and 5-HT concentrations in the range of 0.1–1300.0 and 1.0–650.0 μM, respectively. The applicability of the modified electrode was demonstrated by simultaneous determination of IP and 5-HT in human serum

  1. New fluorescence spectroscopic method for the simultaneous determination of alkaloids in aqueous extract of green coffee beans.

    Science.gov (United States)

    Yisak, Hagos; Redi-Abshiro, Mesfin; Chandravanshi, Bhagwan Singh

    2018-05-11

    There is no fluorescence spectroscopic method for the determination of trigonelline and theobromine in green coffee beans. Therefore, the objective of this study was to develop a new fluorescence spectroscopic method to determine the alkaloids simultaneously in the aqueous extract of green coffee beans. The calibration curves were linear in the range 2-6, 1-6, 1-5 mg/L for caffeine, theobromine and trigonelline, respectively, with R 2  ≥ 0.9987. The limit of detection and limit of quantification were 2, 6 and 7 µg/L and 40, 20 and 20 µg/L for caffeine, theobromine and trigonelline, respectively. Caffeine and trigonelline exhibited well separated fluorescence excitation spectra and therefore the two alkaloids were selectively quantified in the aqueous extract of green coffee. While theobromine showed overlapping fluorescence excitation spectra with caffeine and hence theobromine could not be determined in the aqueous extract of green coffee beans. The amount of caffeine and trigonelline in the three samples of green coffee beans were found to be 0.95-1.10 and 1.00-1.10% (w/w), respectively. The relative standard deviations (RSD ≤ 4%) of the method for the three compounds of interest were of very good. The accuracy of the developed analytical method was evaluated by spiking standard caffeine and trigonelline to green coffee beans and the average recoveries were 99 ± 2% for both the alkaloids. A fast, sensitive and reliable fluorescence method for the simultaneous determination of caffeine and trigonelline in the aqueous extract of green coffee beans was developed and validated. The developed method reflected an effective performance to the direct determination of the two alkaloids in the aqueous extract of green coffee beans.

  2. Simultaneous electrochemical determination of dopamine and paracetamol on multiwalled carbon nanotubes/graphene oxide nanocomposite-modified glassy carbon electrode.

    Science.gov (United States)

    Cheemalapati, Srikanth; Palanisamy, Selvakumar; Mani, Veerappan; Chen, Shen-Ming

    2013-12-15

    In the present study, multiwalled carbon nanotubes (MWCNT)/graphene oxide (GO) nanocomposite was prepared by homogenous dispersion of MWCNT and GO and used for the simultaneous voltammetric determination of dopamine (DA) and paracetamol (PA). The TEM results confirmed that MWCNT walls were wrapped well with GO sheets. The MWCNT/GO nanocomposite showed superior electrocatalytic activity towards the oxidation of DA and PA, when compared with either pristine MWCNT or GO. The major reason for the efficient simultaneous detection of DA and PA at nanocomposite was the synergistic effect between MWCNT and GO. The electrochemical oxidation of DA and PA was investigated by cyclic voltammetry, differential pulse voltammetry and amperometry. The nanocomposite modified electrode showed electrocatalytic oxidation of DA and PA in the linear response range from 0.2 to 400 µmol L(-1) and 0.5 to 400 µmol L(-1) with the detection limit of 22 nmol L(-1) and 47 nmol L(-1) respectively. The proposed sensor displayed good selectivity, sensitivity, stability with appreciable consistency and precision. © 2013 Elsevier B.V. All rights reserved.

  3. Simultaneous determination of mycophenolate mofetil and its active metabolite, mycophenolic acid, by differential pulse voltammetry using multi-walled carbon nanotubes modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Madrakian, Tayyebeh, E-mail: madrakian@basu.ac.ir; Soleimani, Mohammad; Afkhami, Abbas

    2014-09-01

    A highly sensitive electrochemical sensor for the simultaneous determination of mycophenolate mofetil (MPM) and mycophenolic acid (MPA) was fabricated by multi-walled carbon nanotubes modified glassy carbon electrode (MWCNTs/GCE). The electrochemical behavior of these two drugs was studied at the modified electrode using cyclic voltammetry and adsorptive differential pulse voltammetry. MPM and MPA were oxidized at the GCE during an irreversible process. DPV analysis showed two oxidation peaks at 0.87 V and 1.1 V vs. Ag/AgCl for MPM and an oxidation peak at 0.87 V vs. Ag/AgCl for MPA in phosphate buffer solution of pH 5.0. The MWCNTs/GCE displayed excellent electrochemical activities toward oxidation of MPM and MPA relative to the bare GCE. The experimental design algorithm was used for optimization of DPV parameters. The electrode represents linear responses in the range 5.0 × 10{sup −6} to 1.6 × 10{sup −4} mol L{sup −1} and 2.5 × 10{sup −6} mol L{sup −1} to 6.0 × 10{sup −5} mol L{sup −1} for MPM and MPA, respectively. The detection limit was found to be 9.0 × 10{sup −7} mol L{sup −1} and 4.0 × 10{sup −7} mol L{sup −1} for MPM and MPA, respectively. The modified electrode showed a good sensitivity and stability. It was successfully applied to the simultaneous determination of MPM and MPA in plasma and urine samples. - Highlights: • A new modified electrochemical sensor was constructed and used. • Multiwalled carbon nanotubes were used as the modifiers. • MPM and MPA were measured simultaneously at the low levels. • The sensor was used to the determination of MPA and MPM in real samples.

  4. Simultaneous in-line concentration for spectrophotometric determination of cations and anions

    Directory of Open Access Journals (Sweden)

    Rocha Fábio R. P

    2004-01-01

    Full Text Available A flow system is proposed for simultaneous in-line concentration of cations and anions. A sliding-bar commutator was employed to insert an anion and a cation exchange column into a flowing sample stream for serial retention of the analytes. In the injector alternative position, different solutions flowed through the columns for parallel elution of the species in different analytical paths. Three-way solenoid valves allowed the intermittent reagent introduction in the sample zones. Signals were measured by employing two flow-through LED-based detectors. The simultaneous retention of the sample zones in coiled reactors can be also performed to increase the residence time and the analyte conversion rate. The analytical potentiality was demonstrated by the in-line concentration of ammonium and phosphate followed by spectrophotometric detection. For a 90 s loading time, the sampling rate was estimated as 40 determinations per hour, which is three-fold higher than the obtained without performing the tasks simultaneously. Enrichment factors of 8.0 and 18 were estimated for phosphate and ammonium, respectively, yielding detection limits of 1 mg L-1 PO4(3- and 1 mg L-1 NH4+ (99.7% confidence level. The reagent consumption was lower than 2 mg per determination. Results for freshwater samples agreed with the obtained by reference APHA procedures at the 95% confidence level.

  5. Temperature-sensitive microemulsion gel: an effective topical delivery system for simultaneous delivery of vitamins C and E.

    Science.gov (United States)

    Rozman, Branka; Zvonar, Alenka; Falson, Francoise; Gasperlin, Mirjana

    2009-01-01

    Microemulsions (ME)--nanostructured systems composed of water, oil, and surfactants--have frequently been used in attempts to increase cutaneous drug delivery. The primary objective addressed in this work has been the development of temperature-sensitive microemulsion gel (called gel-like ME), as an effective and safe delivery system suitable for simultaneous topical application of a hydrophilic vitamin C and a lipophilic vitamin E. By changing water content of liquid o/w ME (o/w ME), a gel-like ME with temperature-sensitive rheological properties was formed. The temperature-driven changes in its microstructure were confirmed by rotational rheometry, viscosity measurements, and droplet size determination. The release studies have shown that the vitamins' release at skin temperature from gel-like ME were comparable to those from o/w ME and were much faster and more complete than from o/w ME conventionally thickened with polymer (o/w ME carbomer). According to effectiveness in skin delivery of both vitamins, o/w ME was found the most appropriate, followed by gel-like ME and by o/w ME carbomer, indicating that no simple correlation between vitamins release and skin absorption could be found. The cytotoxicity studies revealed good cell viability after exposure to ME and confirmed all tested microemulsions as nonirritant.

  6. First report on hemoglobin electrostatic immobilization on WO3 nanoparticles: application in the simultaneous determination of levodopa, uric acid, and folic acid.

    Science.gov (United States)

    Ghodsi, Javad; Rafati, Amir Abbas; Shoja, Yalda

    2016-05-01

    This work describes the first report about the simultaneous determination of levodopa (L-DOPA) with folic acid (FA) and uric acid (UA) based on electrocatalytic oxidation of L-DOPA with peroxidase properties of hemoglobin (Hb) in the presence of H2O2 as Hb activator. Bovine Hb was electrostatically immobilized on WO3 nanoparticles (WO3NPs) in pH between Hb and WO3NP isoelectric points, and subsequently, a carbon paste electrode (CPE) was modified with the obtained WO3NPs-Hb and multiwalled carbon nanotubes (MWCNTs). The resulting biosensor supplied a sensitive and suitably stable biosensor for the simultaneous determination of L-DOPA, UA, and FA. The obtained linear range and detection limit for L-DOPA, UA, and FA were completely acceptable, and the biosensor response time for these molecules was relatively short so that it reaches about 95 % of its maximum response in less than 10 s. The applicability of the current biosensor was confirmed with the determination of L-DOPA in the presence of fixed amounts of FA and UA in some real samples by the standard addition method.

  7. Simultaneous determination of 15 phenolic constituents of Chinese black rice wine by HPLC-MS/MS with SPE.

    Science.gov (United States)

    Wang, Yutang; Liu, Yuanyuan; Xiao, Chunxia; Liu, Laping; Hao, Miao; Wang, Jianguo; Liu, Xuebo

    2014-06-01

    This study established a new method for quantitative and qualitative determination of certain components in black rice wine, a traditional Chinese brewed wine. Specifically, we combined solid-phase extraction and high-performance liquid chromatography (HPLC) with triple quadrupole mass spectrometry (MS/MS) to determine 8 phenolic acids, 3 flavonols, and 4 anthocyanins in black rice wine. First, we clean samples with OASIS HLB cartridges and optimized extraction parameters. Next, we performed separation on a SHIM-PACK XR-ODS column (I.D. 3.0 mm × 75 mm, 2.2 μm particle size) with a gradient elution of 50% aqueous acetonitrile (V/V) and water, both containing 0.2% formic acid. We used multiple-reaction monitoring scanning for quantification, with switching electrospray ion source polarity between positive and negative modes in a single chromatographic run. We detected 15 phenolic compounds properly within 38 min under optimized conditions. Limits of detection ranged from 0.008 to 0.030 mg/L, and average recoveries ranged from 60.8 to 103.1% with relative standard deviation ≤8.6%. We validated the method and found it to be sensitive and reliable for quantifying phenolic compounds in rice wine matrices. This study developed a new, reliable HPLC-MS/MS method for simultaneous determination of 15 bioactive components in black rice wine. This method was validated and found to be sensitive and reliable for quantifying phenolic compounds in rice wine. © 2014 Institute of Food Technologists®

  8. [Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

    Science.gov (United States)

    Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

    2011-02-01

    A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

  9. Simultaneous DPV determination of morphine and codeine using dsDNA modified screen printed electrode strips coupled with electromembrane extraction

    Directory of Open Access Journals (Sweden)

    Rouhollah Feizbakhsh

    2016-01-01

    Full Text Available In this work a sensitive electrochemical sensor for simultaneous determination of morphine and codeine constructed by application of disposable screen printed carbon electrode strips (SPCE modified by double strand (ds calf thymus DNA. According to the results of the modified SPCE strips and experimented parameters, we observed a considerable shift between potentials of morphine and codeine current peaks. Related to these observed shifts, we studied on the effect of the concentration of modifier and pH value on the anodic oxidation pattern of morphine and codeine in the case of optimize the method to get better signals with maximum potential distance. Also to boosting the LODs of this electroanalytical method coupled with an electro-membrane preconcentration (EME step. The calibration curve which was plotted by the variation of differential pulse voltammetry (DPV currents as a function of different morphine and codeine concentration were linear within the range of 0.7– 40 µM and 2.3- 40 µM for morphine and codeine respectively. Also the limits of detection were 0.07 µM and 0.23 µM, respectively. Finally, the proposed method was able to determine morphine and codeine simultaneously and effectively in urinary real samples

  10. Ultra-performance liquid chromatography tandem mass spectrometry for simultaneous determination of natural steroid hormones in sea lamprey (Petromyzon marinus) plasma and tissues.

    Science.gov (United States)

    Wang, Huiyong; Bussy, Ugo; Chung-Davidson, Yu-Wen; Li, Weiming

    2016-01-15

    This study aims to provide a rapid, sensitive and precise UPLC-MS/MS method for target steroid quantitation in biological matrices. We developed and validated an UPLC-MS/MS method to simultaneously determine 16 steroids in plasma and tissue samples. Ionization sources of Electrospray Ionization (ESI) and Atmospheric Pressure Chemical Ionization (APCI) were compared in this study by testing their spectrometry performances at the same chromatographic conditions, and the ESI source was found up to five times more sensitive than the APCI. Different sample preparation techniques were investigated for an optimal extraction of steroids from the biological matrices. The developed method exhibited excellent linearity for all analytes with regression coefficients higher than 0.99 in broad concentration ranges. The limit of detection (LOD) was from 0.003 to 0.1ng/mL. The method was validated according to FDA guidance and applied to determine steroids in sea lamprey plasma and tissues (fat and testes) by the developed method. Copyright © 2015. Published by Elsevier B.V.

  11. [Simultaneous determination of 7 arsenic species in chicken muscle and chicken liver with high performance liquid chromatography-inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Yang, Lijun; Hu, Qiaoru; Guo, Wei; Liu, Yumin; Song, Xiaohua; Zhang, Pengcheng

    2011-05-01

    A method for the simultaneous determination of 7 arsenic species was developed with high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The sample was extracted with artificial gastric juice. The HPLC separation was performed on an anion analytical column utilizing a gradient elution program of ammonium carbonate and water as the mobile phase. Identification and quantification were achieved by ICP-MS. Good linearities of 7 arsenic species were observed in the range from 1 microg/kg to 50 microg/kg with the correlation coefficients greater than 0.999. The average recoveries of 7 arsenic species spiked at the three levels of 1, 2 and 10 microg/kg ranged from 84.3% to 106.6% with the relative standard deviations of 1.4%-4.2%. The quantification limits of 7 arsenic species were 1 microg/kg. The method was proved to be good reproducibility, high sensitivity and simple preprocessing. This method is suitable for the simultaneous determination of 7 arsenic species in chicken muscle and chicken liver.

  12. Simultaneous determination of seven alkaloids from Rhizoma Corydalis Decumbentis in rabbit aqueous humor by LC-MS/MS: Application to ocular pharmacokinetic studies.

    Science.gov (United States)

    Mao, Zhengsheng; Wang, Xin; Liu, Yangdan; Huang, Yuting; Liu, Youping; Di, Xin

    2017-07-01

    This study aims to establish a fast and sensitive LC-MS/MS method for simultaneous determination of seven alkaloids from Rhizoma Corydalis Decumbentis in rabbit aqueous humor. Aqueous humor samples were processed by protein precipitation and then separated on a Thermo Syncronis C 18 column (50mm×2.1mm, 5μm) with a mobile phase using acetonitrile-0.05% formic acid (28:72, v/v). Detection of the analytes and the internal standard (coptisine) were performed in positive electrospray ionization with selected reaction monitoring. The method showed good linearity (r>0.9931) for all the seven alkaloids. This fully validated method was applied to the studies of aqueous humor pharmacokinetics of seven alkaloids from Rhizoma Corydalis Decumbentis and the effects of borneol on corneal penetration of these alkaloids into aqueous humor. This is the first work that presents a reliable LC-MS/MS method for simultaneous determination of seven alkaloids in rabbit aqueous humor and its application of ocular pharmacokinetics of seven alkaloids from Rhizoma Corydalis Decumbentis. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. A Localized Surface Plasmon Resonance Sensing Method for Simultaneous Determination of Atenolol and Amiloride in Pharmaceutical Dosage Forms and Urine Samples

    Directory of Open Access Journals (Sweden)

    Marwa R. El-Zahry

    2018-01-01

    Full Text Available This contribution describes a simple, fast, and sensitive application of localized surface plasmon resonance effect of silver nanoparticles for simultaneous determination of antihypertensive drugs’ mixture atenolol and amiloride in both pharmaceutical dosage forms and in biological samples (urine. Silver nanoparticles were prepared by chemical reduction of silver nitrate using hydroxylamine HCL in an alkaline medium. Application of silver-hydroxylamine nanoparticles (SH NPs provides many advantages including reproducibility, sensitivity, and cost effective way of analyte determination. Amiloride has four amino groups which act as attachment points on the surface of silver nanoparticles resulting in a synergistic effect on the absorption intensity of atenolol, leading to increase the sensitivity of the determination of both compounds. This method shows excellent advantages comparing with the previously reported methods, including accuracy, precision, and selectivity. The linear range of atenolol is 1 × 10−5–1 × 10−4 mol·L−1 and of amiloride is 1 × 10−6–1 × 10−5 mol·L−1. The limit of detection (LOD values of atenolol and amiloride are 0.89 × 10−5 and 0.42 × 10−6 mol·L−1, respectively.

  14. Simultaneous determination of protein structure and dynamics

    DEFF Research Database (Denmark)

    Lindorff-Larsen, Kresten; Best, Robert B.; DePristo, M. A.

    2005-01-01

    at the atomic level about the structural and dynamical features of proteins-with the ability of molecular dynamics simulations to explore a wide range of protein conformations. We illustrate the method for human ubiquitin in solution and find that there is considerable conformational heterogeneity throughout......We present a protocol for the experimental determination of ensembles of protein conformations that represent simultaneously the native structure and its associated dynamics. The procedure combines the strengths of nuclear magnetic resonance spectroscopy-for obtaining experimental information...... the protein structure. The interior atoms of the protein are tightly packed in each individual conformation that contributes to the ensemble but their overall behaviour can be described as having a significant degree of liquid-like character. The protocol is completely general and should lead to significant...

  15. Spectrophotometric Determination of Iron(II and Cobalt(II by Direct, Derivative, and Simultaneous Methods Using 2-Hydroxy-1-Naphthaldehyde-p-Hydroxybenzoichydrazone

    Directory of Open Access Journals (Sweden)

    V. S. Anusuya Devi

    2012-01-01

    Full Text Available Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH reacts with iron(II and cobalt(II to form reddish-brown and yellow-coloured [Fe(II-HNAHBH] and [Co(II-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II-HNAHBH], Beer’s law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II-HNAHBH] complex obeys Beer’s law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content.

  16. A highly stable and sensitive GO-XDA-Mn2O3 electrochemical sensor for simultaneous electrooxidation of paracetamol and ascorbic acid

    International Nuclear Information System (INIS)

    Ejaz, Ammara; Jeon, Seungwon

    2017-01-01

    Highlights: •π–π interaction of graphene oxide (GO) with 1,4-xylenediamine (XDA) was studied. •The synergistic effect of the Mn 2 O 3 nanospheres with GO-XDA was electrochemically studied in the detection of Paracetamol (PCT) and ascorbic acid (AA). •The GO-XDA-Mn 2 O 3 accurately detected PCT and AA with LOD of 5.6 × 10 −8 M and 6.0 × 10 −7 M respectively. •The GO-XDA-Mn 2 O 3 selectively detected PCT and AA simultaneously in the presence of DA, 5-HT and Glu with peak separation of 240 mV. -- Abstract: Highly stable electrochemical sensor based on strong π- π interactions between GO and XDA was fabricated for simultaneous as well as for individual detection of paracetamol (PCT) and ascorbic acid (AA). The oxidation potential of PCT and AA was greatly resolved with the decoration of Mn 2 O 3 nanospheres. We believe that, presence of metal oxide on the surface of GO-XDA will offer higher electrochemical performance with its large surface area and fast electron transfer ability. Therefore, a comparative study was executed in the presence and absence of Mn 2 O 3 nanospheres on the surface of GO-XDA. The GO-XDA-Mn 2 O 3 modified electrode showed electrocatalytic oxidation of PCT in a very wide linear range of 1 × 10 −6 –1 × 10 −3 M with limit of detection (LOD) and sensitivity of 5.6 × 10 −8 M, 527.04 μAmM −1 cm −2 respectively and AA with 1 × 10 −5 –8 × 10 −3 M linear range, LOD and sensitivity of 6.0 × 10 −7 M, 655.74 μAmM −1 cm −2 respectively. Furthermore, astonishing stability was found when GO-XDA-Mn 2 O 3 nanocomposite was stored for over a week. The proposed sensor displayed incredible selectivity, sensitivity and excellent recovery results for real samples with appreciable consistency and precision suggesting practical utility of the GO-XDA-Mn 2 O 3 as an effective and reliable electrochemical sensor for simultaneous as well as individual determination of PCT and AA.

  17. Development and Validation of a Simultaneous RP-HPLCUV/DAD Method for Determination of Polyphenols in Gels Containing S. terebinthifolius Raddi (Anacardiaceae)

    Science.gov (United States)

    Carvalho, Melina G.; Aragão, Cícero F. S; Raffin, Fernanda N.; de L. Moura, Túlio F. A.

    2017-01-01

    Topical gels containing extracts of Schinus terebinthifolius have been used to treat bacterial vaginosis. It has been reported that this species has antimicrobial, anti-inflammatory and anti-ulcerogenic properties, which can be attributed to the presence of phenolic compounds. In this work, a sensitive and selective reversed-phase HPLC-UV/DAD method for the simultaneous assay of six polyphenols that could be present in S. terebinthifolius was developed. The method was shown to be accurate and precise. Peak purity and similarity index both exceeded 0.99. Calibration curves were linear over the concentration range studied, with correlation coefficients between 0.9931 and 0.9974. This method was used to determine the polyphenol content of a hydroalcoholic extract and pharmacy-compounded vaginal gel. Although the method is useful to assess the 6 phenolic compounds, some compounds could not be detected in the products. SUMMARY A sensitive, selective, accurate and precise reversed-phase HPLC-UV/DAD method for the simultaneous assay of six polyphenols in S. terebinthifolius Raddi Abbreviations used: RP-HPLC-UV/DAD: Reverse Phase High Performance Liquid Chromatograph with Ultraviolet and Diode Array Detector, HPLC: High Performance Liquid Chromatograph, HPLC-UV: High Performance Liquid Chromatograph with Ultraviolet Detector, ANVISA: Brazilian National Health Surveillance Agency, LOD: Limit of detection, LOQ: Limit of quantitation PMID:28539726

  18. Simultaneous Determination of Four Preservatives in Foodstuffs by High Performance Liquid Chromatography

    OpenAIRE

    Mohammad Faraji; Farzaneh Rahbarzare

    2016-01-01

    Background and objectives:  High concentration of preservatives in food may result in gastrointestinal disturbances whereby some patients suffering from asthma, rhinitis, or urticaria. The aim of this study is the introduction and optimization a new method for simultaneous determination of four preservatives (SB, PS, MP, PP) in foodstuff by high performance liquid chromatography. Materials and methods: Important factors in extraction, separation and determination process were optimiz...

  19. Simultaneous electrochemical determination of L-cysteine and L-cysteine disulfide at carbon ionic liquid electrode.

    Science.gov (United States)

    Safavi, Afsaneh; Ahmadi, Raheleh; Mahyari, Farzaneh Aghakhani

    2014-04-01

    A linear sweep voltammetric method is used for direct simultaneous determination of L-cysteine and L-cysteine disulfide (cystine) based on carbon ionic liquid electrode. With carbon ionic liquid electrode as a high performance electrode, two oxidation peaks for L-cysteine (0.62 V) and L-cysteine disulfide (1.3 V) were observed with a significant separation of about 680 mV (vs. Ag/AgCl) in phosphate buffer solution (pH 6.0). The linear ranges were obtained as 1.0-450 and 5.0-700 μM and detection limits were estimated to be 0.298 and 4.258 μM for L-cysteine and L-cysteine disulfide, respectively. This composite electrode was applied for simultaneous determination of L-cysteine and L-cysteine disulfide in two real samples, artificial urine and nutrient broth. Satisfactory results were obtained which clearly indicate the applicability of the proposed electrode for simultaneous determination of these compounds in complex matrices.

  20. Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC-MS/MS.

    Science.gov (United States)

    Hu, Xiaofeng; Hu, Rui; Zhang, Zhaowei; Li, Peiwu; Zhang, Qi; Wang, Min

    2016-09-01

    A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL(-1), and quantitation limits ranged from 0.06 to 0.75 ng mL(-1). Concentration curves were linear from 0.12 to 40 μg kg(-1) with correlation coefficients of R (2) > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria.

  1. Simultaneous all-optical determination of molecular concentration and extinction coefficient.

    Science.gov (United States)

    Cho, Byungmoon; Tiwari, Vivek; Jonas, David M

    2013-06-04

    Absolute molecular number concentration and extinction coefficient are simultaneously determined from linear and nonlinear spectroscopic measurements. This method is based on measurements of absolute femtosecond pump-probe signals. Accounting for pulse propagation, we present a closed form expression for molecular number concentration in terms of absorbance, fluorescence, absolute pump-probe signal, and laser pulse parameters (pulse energy, spectrum, and spatial intensity profile); all quantities are measured optically. As in gravimetric and coulometric determinations of concentration, no standard samples are needed for calibration. The extinction coefficient can then be determined from the absorbance spectrum and the concentration. For fluorescein in basic methanol, the optically determined molar concentrations and extinction coefficients match gravimetric determinations to within 10% for concentrations from 0.032 to 0.540 mM, corresponding to absorbance from 0.06 to 1. In principle, this photonumeric method is extensible to transient chemical species for which other methods are not available.

  2. Method of simultaneous continuous determination of transfer rates of iron and chromium into solution during Fe-Cr alloys dissolution

    International Nuclear Information System (INIS)

    Shirinov, T.I.; Florianovich, G.M.; Skuratnik, Ya.B.

    1978-01-01

    Radiometry method of simultaneous continuous registration of transfer rates of iron and chromium into solution from Fe-Cr alloys with various composition has been developed. Using gamma-spectrometer components of Fe-Cr alloys can be determined with high sensitivity in separate samples according to Fe 59 and Cr 51 radioactive labels, obtained by neutron activation. The above method is applied to estimate Fe and Cr transfer rates into H 2 SO 4 solution at the temperature of 50 deg from Fe - 28% Cr alloy during its active dissolution. It is established, that beginning with some seconds of alloy and solution contact, its components transfer into the solution in the same composition, as in the alloy. The method enables to determine Fe with the accuracy of up to 5% and Cr with that of up to 10%

  3. Simultaneous determination of dapsone, monoacetyldapsone and pyrimethamine in whole blood and plasma by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Lemnge, M M; Rønn, A; Flachs, H

    1993-01-01

    A sensitive, selective and rapid reversed-phase high-performance liquid chromatographic method was developed for the simultaneous analysis of dapsone, monoacetyldapsone and pyrimethamine in human whole blood and plasma. The procedure involved extraction of the compounds and the internal standard...

  4. Simultaneous determination of soil density and moisture by gamma ray attenuation from Cs137 and Am241

    International Nuclear Information System (INIS)

    Barros Ferraz, E.S. de.

    1974-09-01

    The method of simultaneous bulk density and soil moisture determination by attenuation of 241 Am and 137 Cs gamma-radiation is introduced and studied with details. Theoretical considerations are made about the attenuation process in the absorbers, the form of solving the problem of two unknowns; the sensitivity of the method; the influences of the resolution time of the electronic counting equipment, and of the compton scattering in the sample. From the methodological point of view studies are made about the influence of the geometry, adjustment of counting system, choice of radiation sources, attenuation coeficients and the manner of obtaining reliable measurements. It is also presented some applications of the method, its use in soil-water movement studies, in soil profile compaction studies, and specially in swelling soils

  5. Simultaneous determination of radioactive halogen isotopes and 99Tc

    International Nuclear Information System (INIS)

    Kabai, E.; Vajda, N.; Gaca, P.

    2003-01-01

    The purpose of this study was to develop a simplified method for simultaneous determination of radiologically important halogen isotopes and 99 Tc from different types of samples like environmental, biological and waste samples. Due to their long half-lives (longer than 10 5 years) they play important role in the nuclear cycle, especially in environmental monitoring and protection. For a rapid response in the evaluation of 129 I, 36 Cl and 99 Tc contamination levels of these samples it is advantageous to combine the existing individual methods. According to the present procedure, iodine, chlorine and technetium are separated selectively from the same sample aliquot followed by the β spectrometry of the purified fractions. Increased sensitivities can be achieved by neutron activation (NA) especially in the case of 129 I. Our work intends to solve the problem by combining the well-known hot acidic distillation method for iodine separation with the organic extraction process characteristic for technetium separation. The major objective of the work was to separate the disturbing halides from iodine. For this purpose a selective oxidant was applied. For the sample destruction and fractionated distillation an air flow-through installation was used with hot concentrated sulphuric and nitric acids. The trap for iodine contained 3 M NaOH solution. After iodine separation the trap was exchanged for a new one containing the same solution for trapping chlorine or bromine with an addition of 0.01 M KMnO 4 solution as an oxidative agent. As expected, the main part of technetium was contained in the acidic residue after distillation. Tc purification was performed by organic extraction with TBP and TEVA column. (author)

  6. Electrochemical Behavior of Catechol and Hydroquinone at Copper Doped Poly (Methyl Red Coated Hydroxyl Multiwalled Carbon Nanotube Film and Their Simultaneous Determination in Water Samples

    Directory of Open Access Journals (Sweden)

    Ying Zhang

    2014-09-01

    Full Text Available A glassy carbon electrode modified with copper doped poly (methyl red coated hydroxyl multiwalled carbon nanotube film (Cu-PMR/MWCNTs, was developed to serve as a sensor for simultaneous determination of Hydroquinone (HQ and catechol (CC in this paper. The fabricated electrode showed excellent electrocatalytic behaviors towards the oxidation of HQ and CC with the enhancement of the redox peak current and the decrease of the peak-to-peak separation. Under the optimized condition, the individual determination of HQ or CT in their mixtures was performed, the response peak currents of the modified electrodes were linear over ranges of 8.0´10-7~4.0´10-4 M (R2=0.999 for CT and 5.0´10-7~2.0´10-4 M (R2=0.993 for HQ. The sensor also exhibited good sensitivity with the detection limit of 1.0´10-8 mol/L and 5.0´10-8 mol/L for HQ and CT, respectively. The simultaneous determination of HQ and CC was demonstrated by simultaneously changing their concentrations. The reduction peak currents of HQ and CC increased linearly with the concentration of their own in the range of 8´10-7 and 2.0´10-4 M for HQ and CC, with correlation coefficients of 0.994 and 0.995 (S/N=3, respectively. This study provides a new kind of composite modified electrode for electrochemical sensors with good selectivity and strong anti-interference. It has been applied to simultaneous determination of HQ and CT in water sample with high selectivity.

  7. Simultaneous determination of Albendazol and Triclabendazol in Triclazol 22 suspension for veterinary purposes

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M.; Gafas Leyva, Maite; Rosales Bosch, Karina

    2013-01-01

    Triclazol 22 suspension containing triclabendazol and albendazol is used as parasiticide for veterinary purposes. to validate the analytical method for simultaneous determination of triclabendazol and albendazol in triclazol 22 suspension for quality control

  8. Simultaneous determination of metformin and vildagliptin in human plasma by a HILIC-MS/MS method.

    Science.gov (United States)

    Pontarolo, Roberto; Gimenez, Ana Carolina; de Francisco, Thais Martins Guimarães; Ribeiro, Rômulo Pereira; Pontes, Flávia Lada Degaut; Gasparetto, João Cleverson

    2014-08-15

    The objective of this work was to develop and validate a HILIC-MS/MS method for the simultaneous determination of metformin and vildagliptin in human plasma. Chromatographic separation was achieved using an Atlantis HILIC Silica 150-mm × 2.1-mm, 3-μm particle size column maintained at 40°C. The isocratic mobile phase consisted of 20% water and 80% acetonitrile/water solution 95:5 (v/v), containing both 0.1% formic acid and 3mM ammonium formate. The flow rate was maintained at 400 μL min(-1). Data from validation studies demonstrated that the new method is highly selective, sensitive (limits of detection vildagliptin in plasma volunteers who orally received a single dose of metformin (850 mg), vildagliptin (50mg) or drug association (metformin 850 mg+vildagliptin 50mg). The new method can thus also be used as a tool for the clinical monitoring of metformin and vildagliptin. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of antiretroviral drugs in human hair with liquid chromatography-electrospray ionization-tandem mass spectrometry.

    Science.gov (United States)

    Wu, Yan; Yang, Jin; Duan, Cailing; Chu, Liuxi; Chen, Shenghuo; Qiao, Shan; Li, Xiaoming; Deng, Huihua

    2018-04-15

    The determination of the concentrations of antiretroviral drugs in hair is believed to be an important means for the assessment of the long-term adherence to highly active antiretroviral therapy. At present, the combination of tenofovir, lamivudine and nevirapine is widely used in China. However, there was no research reporting simultaneous determination of the three drugs in hair. The present study aimed to develop a sensitive method for simultaneous determination of the three drugs in 2-mg and 10-mg natural hair (Method 1 and Method 2). Hair samples were incubated in methanol at 37 °C for 16 h after being rinsed with methanol twice. The analysis was performed on high performance liquid chromatography tandem mass spectrometry with electronic spray ionization in positive mode and multiple reactions monitoring. Method 1 and Method 2 showed the limits of detection at 160 and 30 pg/mg for tenofovir, at 5 and 6 pg/mg for lamivudine and at 15 and 3 pg/mg for nevirapine. The two methods showed good linearity with the square of correlation coefficient >0.99 at the ranges of 416-5000 and 77-5000 pg/mg for tenofovir, 12-5000 and 15-5000 pg/mg for lamivudine and 39-50,000 and 6-50,000 pg/mg for nevirapine. They gave intra-day and inter-day coefficient of variation <15% and the recoveries ranging from 80.6 to 122.3% and from 83.1 to 114.4%. Method 2 showed LOD and LOQ better than Method 1 for tenofovir and nevirapine and matched Method 1 for lamivudine, but there was high consistency between them in the determination of the three drugs in hair. The population analysis with Method 2 revealed that the concentrations in hair were decreased with the distance of hair segment away from the scalp for the three antiretroviral drugs. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Simultaneous determination of thirteen flavonoids from Xiaobuxin-Tang extract using high-performance liquid chromatography coupled with electrospray ionization mass spectrometry.

    Science.gov (United States)

    Cen, Meifeng; Ruan, Jinxiu; Huang, Lihua; Zhang, Zhenqing; Yu, Nengjiang; Zhang, Youzhi; Cheng, Xuange; Xiong, Xiaohong; Wang, Guixiang; Zang, Linquan; Wang, Sujun

    2015-11-10

    A simple and reliable high performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC-ESI-MS) analysis method was established to simultaneously determine thirteen flavonoids of Xiaobuxing-Tang in intestine perfusate, namely onpordin, 3'-O-methylorobol, glycitein, patuletin, genistein, luteolin, quercetin, nepitrin, quercimeritrin, daidzin, patulitrin, quercetagitrin and 3-glucosylisorhamnetin. Detection was performed on a quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source operating in negative ionization mode. Negative ion ESI was used to form deprotonated molecules at m/z 315 for onpordin, m/z 299 for 3'-O-methylorobol, m/z 283 for glycitein, m/z 331 for patuletin, m/z 269 for genistein, m/z 285 for luteolin, m/z 301 for quercetin, m/z 477 for nepitrin, m/z 463 for quercimeritrin, m/z 461 for daidzin, m/z 493 for patulitrin, m/z 479 for quercetagitrin, m/z 477 for 3-glucosylisorhamnetin and m/z 609.2 for rutin. The linearity, sensitivity, selectivity, repeatability, accuracy, precision, recovery and matrix effect of the assay were evaluated. The proposed method was successfully applied to simultaneous determination of these thirteen flavonoids, and using this method, the intestinal absorption profiles of thirteen flavonoids were preliminarily predicted. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Method for the simultaneous determination of nitrogen, phosphorus and potassium

    International Nuclear Information System (INIS)

    Srapeniants, R.A.; Saveliev, I.B.; Kovtun, J.L.; Sidorov, A.V.; Tsagolov, K.S.

    1980-01-01

    A method for the simultaneous determination of the nitrogen, phosphorus and potassium contents of materials containing them, such as vegetable materials and fertilisers, comprises exposing samples to be analysed and standard samples to neutron irradiation, recording the spectra of gamma radiation induced in the samples, laying the samples aside for a period of time determined by the half-life of the gamma ray-emitting isotopes, again recording the spectra of the samples being analysed and those of the standard samples, superimposing the first and second spectra of the samples being analysed and standard samples and shifting them relative to each other along the energy axis, and determining the content of the elements being analysed by comparing the spectra of the samples being analysed with those of the standard samples. (author)

  12. Simultaneous extractive-photometric determination of Zr and Mo in multicomponent alloys

    International Nuclear Information System (INIS)

    Kutyrev, I.M.; Chernysheva, G.M.; Chebotnikovz, Yu.A.; Basargin, N.N.

    2000-01-01

    Nonaqueous buffer solutions of different acidity are developed for simultaneous photometric determination of Zr and Mo in the extract. Trioctylamine extraction system in toluene - sulfuric acid - molybdenum, zirconium provides selective isolation of the aforementioned elements in one extraction and makes it possible to remove the interfering effect of Fe(2,3), Co(2), Ni(2), Cu(2), Al(3), Ti(4), Cr(3), Mn(2), V(4), Si(4). The reliability of the method is confirmed by determination of the elements in SS123v standard sample [ru

  13. Simultaneous Determination of Binding Constants for Multiple Carbohydrate Hosts in Complex Mixtures

    DEFF Research Database (Denmark)

    Meier, Sebastian; Beeren, Sophie

    2014-01-01

    We describe a simple method for the simultaneous determination of association constants for a guest binding to seven different hosts in a mixture of more than 20 different oligosaccharides. If the binding parameters are known for one component in the mixture, a single NMR titration suffices...

  14. Simultaneous determination of atorvastatin calcium, ezetimibe, and fenofibrate in a tablet formulation by HPLC.

    Science.gov (United States)

    Patel, Archita; Macwana, Chhaya; Parmar, Vishal; Patel, Samir

    2012-01-01

    An accurate, simple, reproducible, and sensitive HPLC method was developed and validated for the simultaneous determination of atorvastatin calcium, ezetimibe, and fenofibrate in a tablet formulation. The analyses were performed on an RP C18 column, 150 x 4.60 mm id, 5 pm particle size. The mobile phase methanol-acetonitrile-water (76 + 13 + 11, v/v/v), was pumped at a constant flow rate of 1 mL/min. UV detection was performed at 253 nm. Retention times of atorvastatin calcium, ezetimibe, and fenofibrate were found to be 2.25, 3.68, and 6.41 min, respectively. The method was validated in terms of linearity, precision, accuracy, LOD, LOQ, and robustness. The response was linear in the range 2-10 microg/mL (r2 = 0.998) for atorvastatin calcium, 2-10 microg/mL (r2 = 0.998) for ezetimibe, and 40-120 microg/mL (r2 = 0.998) for fenofibrate. The developed method can be used for routine quality analysis of the drugs in the tablet formulation.

  15. [Simultaneous determination of five main index components and specific chromatograms analysis in Xiaochaihu granules].

    Science.gov (United States)

    Zhuang, Yan-Shuang; Cai, Hao; Liu, Xiao; Cai, Bao-Chang

    2012-01-01

    Reversed phase high performance liquid chromatography with diode array detector was employed for simultaneous determination of five main index components and specific chromatograms analysis in Xiaochaihu granules with a linear gradient elution of acetonitrile-water (containing 0.1% phosphoric acid) as mobile phase. The results showed that five main index components (baicalin, baicalein, wogonoside, wogonin, enoxolone) were separated well under the analytical condition. The linear ranges of five components were 0.518 - 16.576, 0.069 - 2.197, 0.167 - 5.333, 0.009 - 0.297 and 0.006 - 0.270 mg x g(-1), respectively. The correlation coefficients were 0.999 9, and the average recoveries ranged from 95% to 105%. Twelve common peaks were selected as the specific chromatograms of Xiaochaihu granules with baicalin as the reference peak. There were good similarities between the reference and the ten batches of samples. The similarity coefficients were no less than 0.9. The analytical method established is highly sensitive with strong specificity and it can be used efficiently in the quality control of Xiaochaihu granules.

  16. Simultaneous HPTLC Determination of Rabeprazole and Itopride Hydrochloride From Their Combined Dosage Form

    OpenAIRE

    Suganthi, A.; John, Sofiya; Ravi, T. K.

    2008-01-01

    A simple, precise, sensitive, rapid and reproducible HPTLC method for the simultaneous estimation of the rabeprazole and itopride hydrochloride in tablets was developed and validated. This method involves separation of the components by TLC on precoated silica gel G60F254 plate with solvent system of n-butanol, toluene and ammonia (8.5:0.5:1 v/v/v) and detection was carried out densitometrically using a UV detector at 288 nm in absorbance mode. This system was found to give compact spots for ...

  17. Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

    Directory of Open Access Journals (Sweden)

    Rania N. El-Shaheny

    2015-01-01

    Full Text Available A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO and mebeverine HCl (MBV in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB and MBV degradation product (veratric acid, VER. Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Student t-test and the variance ratio F-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

  18. Simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Gupta, V K; Jain, Rajeev; Lukram, Ojitkumar; Agarwal, Shilpi; Dwivedi, Ashish

    2011-01-15

    A rapid and sensitive liquid chromatography tandem mass spectrometry method has been developed and validated for the simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma. The solid-phase extraction technique was used for the extraction of ramipril, ramiprilat and telmisartan from human plasma. Trandolaprilat and hydrochlorothiazide were used as the internal standards (ISs). Chromatography was performed on a Hypurity C18, 5 μm, 50 mm × 4.6mm column, with the mobile phase consisting of ammonium acetate and acetonitrile (in a 20:80 ratio), followed by detection using mass spectrometry. The method involves a simple reversed isocratic chromatography condition and mass spectrometry detection, which enables detection at sub-nanogram levels. The method was validated and the lower limit of quantification for ramipril, ramiprilat and telmisartan was found to be 0.1 ng mL(-1), 0.1 ng mL(-1) and 2 ng mL(-1), respectively. The mean recovery for ramipril, ramiprilat and telmisartan ranged from 90.1 to 104.1%. This method increased the sensitivity and selectivity; resulting in high-throughput analysis of ramipril, ramiprilat and telmisartan using two different ISs in a single experiment for bioequivalence studies, with a chromatographic run time of 1.5 min only. Copyright © 2010 Elsevier B.V. All rights reserved.

  19. Simultaneous determination of iridoid glycosides, phenethylalcohol glycosides and furfural derivatives in Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass spectrometry

    DEFF Research Database (Denmark)

    Xu, Jun; Wu, Jie; Zhu, Ling-Ying

    2012-01-01

    In this study, a sensitive and selective method for simultaneously quantifying eight major components (four iridoid glycosides, three phenethylalcohol glycosides and one furfural derivative) of Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass spectrom......In this study, a sensitive and selective method for simultaneously quantifying eight major components (four iridoid glycosides, three phenethylalcohol glycosides and one furfural derivative) of Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass...

  20. Simultaneous voltammetric determination of 2-nitrophenol and 4-nitrophenol based on an acetylene black paste electrode modified with a graphene-chitosan composite

    International Nuclear Information System (INIS)

    Deng, Peihong; Xu, Zhifeng; Li, Junhua

    2014-01-01

    We describe a simple and sensitive voltammetric method for the simultaneous determination of 2-nitrophenol and 4-nitrophenol. It is based on the use of an acetylene black paste electrode modified with a graphene-chitosan composite film (denoted as Gr-Chit/ABPE). The reduction peak currents of 2-nitrophenol (at −252 mV) and of 4-nitrophenol (at −340 mV) in pH 1.0 solution increase significantly at the Gr-Chit/ABPE in comparison to a bare ABPE. Factors affecting sensitivity were optimized and a linear relationship is found between peak current and the concentrations of 2-nitrophenol (in the 0.4 μM to 80 μM range) and for 4-nitrophenol (in the 0.1 μM to 80 μM range). The detection limits (at an SNR of 3 and after a 30-s accumulation time) are 200 nM for 2-nitrophenol and 80 nM for 4-nitrophenol, respectively. The modified electrode was successfully applied to the direct and parallel determination of 2-nitrophenol and 4-nitrophenol in spiked water samples. (author)

  1. Simultaneous Absorptance and Thermal-Diffusivity Determination of Optical Components with Laser Calorimetry Technique

    Science.gov (United States)

    Wang, Yanru; Li, Bincheng

    2012-11-01

    The laser calorimetry (LCA) technique is used to determine simultaneously the absorptances and thermal diffusivities of optical components. An accurate temperature model, in which both the finite thermal conductivity and the finite sample size are taken into account, is employed to fit the experimental temperature data measured with an LCA apparatus for a precise determination of the absorptance and thermal diffusivity via a multiparameter fitting procedure. The uniqueness issue of the multiparameter fitting is discussed in detail. Experimentally, highly reflective (HR) samples prepared with electron-beam evaporation on different substrates (BK7, fused silica, and Ge) are measured with LCA. For the HR-coated sample on a fused silica substrate, the absorptance is determined to be 15.4 ppm, which is close to the value of 17.6 ppm, determined with a simplified temperature model recommended in the international standard ISO11551. The thermal diffusivity is simultaneously determined via multiparameter fitting to be approximately 6.63 × 10-7 m2 · s-1 with a corresponding square variance of 4.8 × 10-4. The fitted thermal diffusivity is in reasonably good agreement with the literature value (7.5 × 10-7 m2 · s -1). Good agreement is also obtained for samples with BK7 and Ge substrates.

  2. Spectrophotometric Methods for Simultaneous Determination of Oxytetracycline HCl and Flunixin Meglumine in Their Veterinary Pharmaceutical Formulation

    Directory of Open Access Journals (Sweden)

    Hanan A. Merey

    2017-01-01

    Full Text Available Four precise, accurate, selective, and sensitive UV-spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of Oxytetracycline HCl (OXY and Flunixin Meglumine (FLU. The first method, dual wavelength (DW, depends on measuring the difference in absorbance (ΔA 273.4–327 nm for the determination of OXY where FLU is zero while FLU is determined at ΔA 251.7–275.7 nm. The second method, first-derivative spectrophotometric method (1D, depends on measuring the peak amplitude of the first derivative selectively at 377 and 266.7 nm for the determination of OXY and FLU, respectively. The third method, ratio difference method, depends on the difference in amplitudes of the ratio spectra at ΔP 286.5–324.8 nm and ΔP 249.6–286.3 nm for the determination of OXY and FLU, respectively. The fourth method, first derivative of ratio spectra method (1DD, depends on measuring the amplitude peak to peak of the first derivative of ratio spectra at 296.7 to 369 nm and 259.1 to 304.7 nm for the determination of OXY and FLU, respectively. Different factors affecting the applied spectrophotometric methods were studied. The proposed methods were validated according to ICH guidelines. Satisfactory results were obtained for determination of both drugs in laboratory prepared mixture and pharmaceutical dosage form. The developed methods are compared favourably with the official ones.

  3. Nanomolar simultaneous determination of tryptophan and melatonin by a new ionic liquid carbon paste electrode modified with SnO2-Co3O4@rGO nanocomposite.

    Science.gov (United States)

    Zeinali, Homa; Bagheri, Hasan; Monsef-Khoshhesab, Zahra; Khoshsafar, Hosein; Hajian, Ali

    2017-02-01

    This work describes the development of a new sensor for simultaneous determination of tryptophan and melatonin. The proposed sensor was an ionic liquid carbon paste electrode modified with reduced graphene oxides decorated with SnO 2 -Co 3 O 4 nanoparticles. The voltammetric oxidation of the analytes by the proposed sensor confirmed that the electrooxidation process undergoes a two-electron/one-proton reaction for melatonin and a two-electron/two-proton reaction for tryptophan in diffusion-controlled processes. Moreover, based on the excellent electrochemical properties of the modified electrode, a sensitive voltammetric method was used for individual and simultaneous determination of melatonin and tryptophan in the aqueous solutions. Under the optimized experimental conditions, a linear response obtained in the range of 0.02 to 6.00μmolL -1 with detection limits of 4.1 and 3.2nmolL -1 for melatonin and tryptophan, respectively. The prepared sensor possessed accurate and rapid response toward melatonin and tryptophan with a good sensitivity, selectivity, stability, and repeatability. Finally, the applicability of the proposed sensor was verified by evaluation of melatonin and tryptophan in various real samples including human serum and tablet samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Simultaneous determination of 2,4,6-trichlorophenol and pentachlorophenol based on poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified electrode

    International Nuclear Information System (INIS)

    Zhu, Xiaolin; Zhang, Kexin; Lu, Nan; Yuan, Xing

    2016-01-01

    Graphical abstract: A poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified glassy carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP) without any pretreatment. - Highlights: • A poly(RhB)/graphene oxide/multiwalled carbon nanotubes composite was synthesized. • The composite film was characterized by SEM, XRD, EIS and Raman spectroscopy. • The simultaneous electrochemical determination of 2,4,6-TCP and PCP was realized. • The electrode showed high sensitivity, excellent reproducibility and good stability. • The electrode was used to determine 2,4,6-TCP and PCP in practical water samples. - Abstract: In the present study, a poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes nanocomposite modified glass carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP). The PRhB/GO/MWCNTs film was extensively characterized by emission scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and electrochemical impedance spectroscopy (EIS). The electrochemical behaviors of 2,4,6-TCP and PCP were investigated by cyclic voltammetry, linear sweep voltammetry and differential pulse voltammetry. Due to the synergistic effect, the PRhB/GO/MWCNTs/GCE significantly facilitated the simultaneous electro-oxidation of 2,4,6-TCP and PCP with peak potential difference of 160 mV and enhanced oxidation currents. Under optimum conditions, the oxidation current of 2,4,6-TCP was linear to its concentration in the ranges of 4.0 × 10"−"9 to 1.0 × 10"−"7 M and 1.0 × 10"−"7 to 1.0 × 10"−"4 M with the detection limit (S/N = 3) of 8.0 × 10"−"1"0 M. And the linear concentration ranges for PCP were 2.0 × 10"−"9 to 1.0 × 10"−"7 M and 1.0 × 10"−"7 to 9.0 × 10"−"5 M with the detection limit of 5.0 × 10"−"1"0 M

  5. Simultaneous determination of 2,4,6-trichlorophenol and pentachlorophenol based on poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Xiaolin; Zhang, Kexin; Lu, Nan; Yuan, Xing, E-mail: yuanx@nenu.edu.cn

    2016-01-15

    Graphical abstract: A poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified glassy carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP) without any pretreatment. - Highlights: • A poly(RhB)/graphene oxide/multiwalled carbon nanotubes composite was synthesized. • The composite film was characterized by SEM, XRD, EIS and Raman spectroscopy. • The simultaneous electrochemical determination of 2,4,6-TCP and PCP was realized. • The electrode showed high sensitivity, excellent reproducibility and good stability. • The electrode was used to determine 2,4,6-TCP and PCP in practical water samples. - Abstract: In the present study, a poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes nanocomposite modified glass carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP). The PRhB/GO/MWCNTs film was extensively characterized by emission scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and electrochemical impedance spectroscopy (EIS). The electrochemical behaviors of 2,4,6-TCP and PCP were investigated by cyclic voltammetry, linear sweep voltammetry and differential pulse voltammetry. Due to the synergistic effect, the PRhB/GO/MWCNTs/GCE significantly facilitated the simultaneous electro-oxidation of 2,4,6-TCP and PCP with peak potential difference of 160 mV and enhanced oxidation currents. Under optimum conditions, the oxidation current of 2,4,6-TCP was linear to its concentration in the ranges of 4.0 × 10{sup −9} to 1.0 × 10{sup −7} M and 1.0 × 10{sup −7} to 1.0 × 10{sup −4} M with the detection limit (S/N = 3) of 8.0 × 10{sup −10} M. And the linear concentration ranges for PCP were 2.0 × 10{sup −9} to 1.0 × 10{sup −7} M and 1.0 × 10{sup −7} to 9.0 × 10{sup −5} M with the

  6. Mercury-free simultaneous determination of cadmium and lead at a glassy carbon electrode modified with multi-wall carbon nanotubes

    International Nuclear Information System (INIS)

    Wu Kangbing; Hu Shengshui; Fei Junjie; Bai Wen

    2003-01-01

    A multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE) was described for the simultaneous determination of trace levels of cadmium and lead by anodic stripping voltammetry (ASV). In pH 4.5 NaAc-HAc buffer containing 0.02 mol/l KI, Cd 2+ and Pb 2+ first adsorb onto the surface of a MWNT film coated GCE and then reduce at -1.20 V. During the positive potential sweep, reduced cadmium and lead were oxidized, and two well-defined stripping peaks appeared at -0.88 and -0.62 V. Compared with a bare GCE, a MWNT film coated GCE greatly improves the sensitivity of determining cadmium and lead. Low concentration of I - significantly enhances the stripping peak currents since it induces Cd 2+ and Pb 2+ to adsorb at the electrode surface. The striping peak currents change linearly with the concentration of Cd 2+ from 2.5x10 -8 to 1x10 -5 mol/l and with that of Pb 2+ from 2x10 -8 to 1x10 -5 mol/l. The lowest detectable concentrations of Cd 2+ and Pb 2+ are estimated to be 6x10 -9 and 4x10 -9 mol/l, respectively. The high sensitivity, selectivity, and stability of this MWNT film coated electrode demonstrated its practical application for a simple, rapid and economical determination of trace levels of Cd 2+ and Pb 2+ in water samples

  7. Rapid Multisample Analysis for Simultaneous Determination of Anthropogenic Radionuclides in Marine Environment

    DEFF Research Database (Denmark)

    Qiao, Jixin; Shi, Keliang; Hou, Xiaolin

    2014-01-01

    An automated multisample processing flow injection (FI) system was developed for simultaneous determination of technetium, neptunium, plutonium, and uranium in large volume (200 L) seawater. Ferrous hydroxide coprecipitation was used for the preliminary sample treatment providing the merit of sim...... reliable data with reduced analytical cost in both radioecology studies and nuclear emergency preparedness....

  8. Simultaneous determination of a binary mixture of pantoprazole sodium and itopride hydrochloride by four spectrophotometric methods

    Science.gov (United States)

    Ramadan, Nesrin K.; El-Ragehy, Nariman A.; Ragab, Mona T.; El-Zeany, Badr A.

    2015-02-01

    Four simple, sensitive, accurate and precise spectrophotometric methods were developed for the simultaneous determination of a binary mixture containing Pantoprazole Sodium Sesquihydrate (PAN) and Itopride Hydrochloride (ITH). Method (A) is the derivative ratio method (1DD), method (B) is the mean centering of ratio spectra method (MCR), method (C) is the ratio difference method (RD) and method (D) is the isoabsorptive point coupled with third derivative method (3D). Linear correlation was obtained in range 8-44 μg/mL for PAN by the four proposed methods, 8-40 μg/mL for ITH by methods A, B and C and 10-40 μg/mL for ITH by method D. The suggested methods were validated according to ICH guidelines. The obtained results were statistically compared with those obtained by the official and a reported method for PAN and ITH, respectively, showing no significant difference with respect to accuracy and precision.

  9. Simultaneous quantitative determination of multiple bioactive markers in Ocimum sanctum obtained from different locations and its marketed herbal formulations using UPLC-ESI-MS/MS combined with principal component analysis.

    Science.gov (United States)

    Pandey, Renu; Chandra, Preeti; Srivastava, Mukesh; Mishra, D K; Kumar, Brijesh

    2015-01-01

    Ocimum sanctum L., with phenolic acids, flavonoids, propenyl phenols and terpenoids as active pharmacological constituents, is a popular medicinal herb and is present as an ingredient in many herbal formulations. Therefore, development of a reliable analytical method for simultaneous determination of the pharmacologically active constituents of O. sanctum is of high importance. To develop and validate a new, rapid, sensitive and selective UPLC-ESI/MS/MS method for simultaneous determination of 23 bioactive markers including phenolic acids, flavonoids, propenyl phenol and terpenoid in the leaf extract and marketed herbal formulations of O. sanctum. An UPLC-ESI/MS/MS method using negative electrospray ionisation (ESI) in multiple-reaction-monitoring (MRM) mode was used for simultaneous determination. Chromatographic separation was achieved on an Acquity UPLC BEH C18 -column using a gradient elution with 0.1% formic acid in water and 0.1% formic acid in acetonitrile. Principal component analysis (PCA) was applied to correlate and discriminate eight geographical collections of O. sanctum based on quantitative data of the analytes. The developed method was validated as per International Conference on Harmonization guidelines and found to be accurate, with overall recovery in the range 95.09-104.84% (RSD ≤ 1.85%), precise (RSD ≤ 1.98%) and linear (r(2)  ≥ 0.9971) over the concentration range of 0.5-1000 ng/mL. Ursolic acid was found to be the most abundant marker in all the samples investigated, except for the marketed tablet. The method established is simple, rapid and sensitive, hence it can be reliably utilised for the quality control of O. sanctum and derived herbal formulations. Copyright © 2015 John Wiley & Sons, Ltd.

  10. One-shot flow injection spectrophotometric simultaneous determination of copper, iron and zinc in patients' sera with newly developed multi-compartment flow cell

    International Nuclear Information System (INIS)

    Teshima, Norio; Gotoh, Shingo; Ida, Kazunori; Sakai, Tadao

    2006-01-01

    We propose here an affordable flow injection method for simultaneous spectrophotometric determination of copper, iron and zinc in patients' sera. The use of a newly designed multi-compartment flow cell allowed the simultaneous determination of the three metals with a single injection ('one-shot') and a double beam spectrophotometer. The chemistry relied on the reactions of these metals with 2-(5-nitro-2-pyridylazo)-5-[N-propyl-N-(3-sulfopropyl)amino]phenol (nitro-PAPS) to form corresponding colored complexes. At pH 3.8, only copper-nitro-PAPS complex was formed in the presence of pyrophosphate as a masking agent for iron, and then the copper and iron(II) complexes were formed in the presence of reductant (ascorbic acid) at the same pH, and finally all three metals reacted with nitro-PAPS at pH 8.6. The characteristics were introduced into the flow system to determine each metal selectively and sensitively. Under the optimum conditions, linear calibration curves for the three metals were obtained in the range of 0.01-1 mg L -1 with a sample throughput rate of 20 h -1 . The limits of detection (3σ) were 3.9 μg L -1 for copper, 4.1 μg L -1 for iron and 4.0 μg L -1 for zinc. The proposed method was applied to analysis of some patients' sera

  11. SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS ESTIMATION OF TOLPERISONE HYDROCHLORIDE AND DICLOFENAC SODIUM IN SYNTHETIC MIXTURE

    OpenAIRE

    Patel Satish A; Hariyani Kaushik P

    2012-01-01

    The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of Diclofenac sodium and Tolperisone hydrochloride in bulk and synthetic mixture. The method is based on the simultaneous equations for analysis of both the drugs using methanol as solvent. Diclofenac sodium has absorbance maxima at 281 nm and Tolperisone hydrochloride has absorbance maxima at 255 nm in methanol. The linearity was obtained in...

  12. SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS ESTIMATION OF EPERISONE HYDROCHLORIDE AND DICLOFENAC SODIUM IN SYNTHETIC MIXTURE

    OpenAIRE

    Patel Paresh U; Patel Sejal K; Patel Umang J

    2012-01-01

    The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of diclofenac sodium and Eperisone hydrochloride in bulk and synthetic mixture. The method is based on the simultaneous equations for analysis of both the drugs using methanol as solvent. Diclofenac sodium has absorbance maxima at 281 nm and Eperisone hydrochloride has absorbance maxima at 255 nm in methanol. The linearity was obtained in the...

  13. Simultaneous determination of triple therapy for Helicobacter pylori in human plasma by reversed phase chromatography with online wavelength switching

    Science.gov (United States)

    Ahmed, Sameh; Atia, Noha N.

    2015-02-01

    The infection of gastric mucosa by Helicobacter pylori (HP) is an essential cofactor in the aetiology of gastroduodenal ulcer and gastric carcinoma. Because of the bacterial resistance, combination therapy containing omeprazole (OME), tinidazole (TNZ) and clarithromycin (CLA) is commonly used for eradication of HP. However, the simultaneous determination of the triple therapy in human plasma was not reported. A simple, reproducible, and selective HPLC method was developed for the simultaneous determination of the triple therapy mixture used for management of HP infections in human plasma. An HPLC procedure based on a liquid-liquid extraction, enrichment of the analytes and subsequent reversed-phase chromatography with UV detection was used. To enable sensitive and selective detection, the method involved the use of online wavelength switching detection, with two different detection wavelengths; 280 nm for detection of OME and TNZ and 210 nm for detection of CLA. Separations were performed on C18 analytical column with acetonitrile-10 mM phosphate buffer of pH = 3.0 at flow rate of 1.0 mL min-1. The linear ranges in human plasma were 0.05-10 μg mL-1 with correlation coefficients >0.9990. The detection limits in human plasma were 0.02-0.07 μg mL-1. Validation parameters were assessed in compliance with US-FDA guidelines. The method proved to be valuable for the therapeutic drug monitoring after oral administration of triple therapy tablets.

  14. Simultaneous determination of quinolones for veterinary use by high-performance liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Rodríguez Cáceres, M I; Guiberteau Cabanillas, A; Galeano Díaz, T; Martínez Cañas, M A

    2010-02-01

    A selective method based on high-performance liquid chromatography with electrochemical detection (HPLC-ECD) has been developed to enable simultaneous determination of three fluoroquinolones (FQs), namely danofloxacin (DANO), difloxacin (DIFLO) and sarafloxacin (SARA). The fluoroquinolones are separated on a Novapack C-18 column and detected in a high sensitivity amperometric cell at a potential of +0.8 V. Solid-phase extraction was used for the extraction of the analytes in real samples. The range of concentration examined varied from 10 to 150 ng g(-1) for danofloxacin, from 25 to 100 ng g(-1) for sarafloxacin and from 50 to 315 ng g(-1) for difloxacin, respectively. The method presents detection limits under 10 ng g(-1) and recoveries around 90% for the three analytes have been obtained in the experiments with fortified samples. This HPLC-ECD approach can be useful in the routine analysis of antibacterial residues being less expensive and less complicated than other more powerful tools as hyphenated techniques. 2009 Elsevier B.V. All rights reserved.

  15. Simultaneous determination of sulpiride and mebeverine by HPLC method using fluorescence detection: application to real human plasma

    Directory of Open Access Journals (Sweden)

    Walash Mohamed I

    2012-02-01

    Full Text Available Abstract A new simple, rapid and sensitive reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of sulpiride (SUL and mebeverine Hydrochloride (MEB in the presence of their impurities and degradation products. The separation of these compounds was achieved within 6 min on a 250 mm, 4.6 mm i.d., 5 m particle size Waters®-C18 column using isocractic mobile phase containing a mixture of acetonitrile and 0.01 M dihydrogenphosphate buffer (45:55 at pH = 4.0. The analysis was performed at a flow rate of 1.0 mL/min with fluorescence-detection at excitation 300 nm and emission at 365 nm. The concentration-response relationship was linear over a concentration range of 10- 100 ng/mL for both MEB and SUL with a limit of detection 0.73 ng/mL and 0.85 ng/mL for MEB and SUL respectively. The proposed method was successfully applied for the analysis of both MEB and SUL in bulk with average recoveries of 100.22 ± 0.757% and 99.96 ± 0.625% respectively, and in commercial tablets with average recoveries of 100.04 ± 0.93% and 100.03 ± 0.376% for MEB and SUL respectively. The proposed method was successfully applied to the determination of MEB metabolite (veratic acid in real plasma simultaneously with SUL. The mean% recoveries (n = 3 for both MEB metabolite (veratic acid and SUL were 100.36 ± 2.92 and 99.06 ± 2.11 for spiked human plasma respectively. For real human plasma, the mean% recoveries (n = 3 were and respectively.

  16. Simultaneous Determination of 13 Anticoagulant Rodenticidesin Human Blood by Liquid Chromatography-Tandem Mass Spectrometry and its Application in Three Poisoning Cases.

    Science.gov (United States)

    Qiao, Zheng; Xiang, Ping; Shen, Baohua; Shen, Min; Yan, Hui

    2018-05-01

    Anticoagulant rodenticides are widely used for rodent control around the world. A rapid and sensitive method was developed and validated for the simultaneous determination of 13 anticoagulant rodenticides (coumafuryl, pindone, valone, warfarin, coumatetralyl, coumachlor, diphacinone, dicumarol, chlorophacinone, bromadiolone, difenacoum, flocoumafen, and brodifacoum) in human blood by liquid chromatography-tandem mass spectrometry. After liquid-liquid extraction, the anticoagulant rodenticides were separated on an Eclipse Plus C18 column. Linearities were observed for each analyte in blood ranging from 0.5 to 50 ng/mL, with correlation coefficients over 0.99. The limits of detection ranged from 0.01 to 0.2 ng/mL, and the limits of quantification were 0.5 ng/mL for all analytes. The intraday and interday precisions were <15%, and accuracies ranged from 80.3% to 111.0%. This validated method with high sensitivity has been applied in three anticoagulant rodenticide poisoning cases and has been used successfully in monitoring blood concentrations for months. © 2017 American Academy of Forensic Sciences.

  17. Different Chromatographic Methods for Simultaneous Determination of Mefenamic Acid and Two of Its Toxic Impurities.

    Science.gov (United States)

    Morcoss, Martha M; Abdelwahab, Nada S; Ali, Nouruddin W; Elsaady, Mohammed T

    2017-08-01

    Two sensitive, accurate and precise chromatographic methods mentioned as TLC-densitometric method and RP-HPLC-DAD method, were developed and validated for the simultaneous determination of mefenamic acid (MEF) and its two toxic impurities, benzoic acid (BA) and 2,3-dimethylaniline (DMA). In the proposed TLC-densitometric method a developing system consisting of chloroform:acetone:acetic acid:ammonia solution(70:30:2:2, v/v/v/v) was used, TLC aluminum plates 60 F254 was used as a stationary phase and the separated bands were UV-scanned at 225 nm. While the proposed RP-HPLC-DAD method depended on chromatographic separation on C18 column using 0.05 M KH2PO4 buffer: acetonitrile (40:60, v/v) as a mobile phase at constant flow rate of 1 mL/min with UV detection at 225 nm. Linear relationships were obtained in the ranges of 0.3-2, 0.3-2 and 0.3-1.8 μg/band (for TLC-densitometric method) and in the ranges of 7-50, 10-50 and 7-50 μg/mL (for HPLC-DAD method) for MEF, BA and DMA, respectively. Factors affecting the developed methods have been studied and optimized. Moreover ,the proposed methods were successfully applied for determination of the studied drug in its pharmaceutical dosage form. The methods showed no significance difference when compared with the reported method using F-test and Student's-t test. The low of detection and quantization limits of the proposed methods get them suitable for quality control and stability studies of MEF in pharmaceutical formulation. The developed methods have advantages of being more selective and sensitive than the published methods. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  18. Spectrophotometric simultaneous determination of Rabeprazole Sodium and Itopride Hydrochloride in capsule dosage form

    Science.gov (United States)

    Sabnis, Shweta S.; Dhavale, Nilesh D.; Jadhav, Vijay. Y.; Gandhi, Santosh V.

    2008-03-01

    A new simple, economical, rapid, precise and accurate method for simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form has been developed. The method is based on ratio spectra derivative spectrophotometry. The amplitudes in the first derivative of the corresponding ratio spectra at 231 nm (minima) and 260 nm were selected to determine rabeprazole sodium and itopride hydrochloride, respectively. The method was validated with respect to linearity, precision and accuracy.

  19. Net Analyte Signal Standard Additions Method for Simultaneous Determination of Sulfamethoxazole and Trimethoprim in Pharmaceutical Formulations and Biological Fluids

    Directory of Open Access Journals (Sweden)

    M. H. Givianrad

    2012-01-01

    Full Text Available The applicability of a novel net analyte signal standard addition method (NASSAM to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim was verified by UV-visible spectrophotometry. The results confirmed that the net analyte signal standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. Moreover, applying the net analyte signal standard additions method revealed that the two drugs could be determined simultaneously with the concentration ratios of sulfamethoxazole to trimethoprim varying from 1:35 to 60:1 in the mixed samples. In addition, the limits of detections were 0.26 and 0.23 μmol L-1 for sulfamethoxazole and trimethoprim, respectively. The proposed method has been effectively applied to the simultaneous determination of sulfamethoxazole and trimethoprim in some synthetic, pharmaceutical formulation and biological fluid samples.

  20. Simultaneous determination of telmisartan and amlodipine in dog plasma by LC-MS-MS.

    Science.gov (United States)

    Wang, Baolian; Sheng, Li; Li, Yan

    2015-01-01

    A simple, rapid and sensitive method was established for the simultaneous determination of telmisartan and amlodipine in dog plasma by a HPLC-MS-MS analysis. The plasma sample preparation was a simple deproteinization by the addition of three volumes of methanol/acetonitrile mixture followed by centrifugation. The analytes and internal standard diphenhydramine were separated on a Zorbax SB-C18 column with a mobile phase of acetonitrile : water (45 : 55, v/v) at a flow rate of 0.2 mL/min with an operating temperature of 25°C. Detection was carried out by electrospray ionization in positive-ion multiple reaction monitoring mode. The calibration plots in dog plasma were linear over the ranges of 0.5-2,000 ng/mL for telmisartan and 0.5-500 ng/mL for amlodipine. The lower limit of quantification was 0.5 ng/mL for two analytes. The intra- and interday precisions (RSD%) were within 9.0%. The average recoveries of analytes were >85.0%. The method was successfully applied to the pharmacokinetic study of the two compounds after oral administration of telmisartan-amlodipine combination preparation to dogs. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  1. Sequential injection approach for simultaneous determination of ultratrace plutonium and neptunium in urine with accelerator mass spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    An analytical method was developed for simultaneous determination of ultratrace level plutonium (Pu) and neptunium (Np) using iron hydroxide coprecipitation in combination with automated sequential injection extraction chromatography separation and accelerator mass spectrometry (AMS) measurement...... show that preboiling and aging are important for obtaining high chemical yields for both Pu and Np, which is possibly related to the aggregation and adsorption behavior of organic substances contained in urine. Although the optimal condition for Np and Pu simultaneous determination requires 5-day aging...

  2. One-step electrochemical approach for the preparation of graphene wrapped-phosphotungstic acid hybrid and its application for simultaneous determination of sunset yellow and tartrazine

    International Nuclear Information System (INIS)

    Gan Tian; Sun Junyong; Cao Shuqin; Gao Fuxing; Zhang Yuxia; Yang Yingqin

    2012-01-01

    Highlights: ► Graphene layer–wrapped PTA hybrid is one–step electropolymerized onto GCE surface. ► Graphene–PTA/GCE is used for simultaneous detection of sunset yellow and tartrazine. ► The oxidation mechanisms of sunset yellow and tartrazine were studied. ► Sunset yellow and tartrazine contents in soft drink samples are successfully determined. - Abstract: We have demonstrated a one-step and effective electrochemical method to prepare graphene (GN) layer-wrapped phosphotungstic acid (PTA) hybrid on the surface of glassy carbon electrode (GCE) using graphene as an electron transfer mediator. The PTA coupled with graphene provides good selectivity and high sensitivity for the simultaneous determination of two synthetic food colorants, sunset yellow and tartrazine, exhibiting as well-defined oxidation peaks in differential pulse voltammetry with a peak potential separation of ca. 260 mV. The detection limit was found to be 0.5 μg L −1 for sunset yellow and 30.0 μg L −1 for tartrazine. The interference of some common food additives was studied and it was concluded that application of this method for the determination of sunset yellow and tartrazine in several commercial soft drink samples led to satisfactory results. This study provides useful further evidences for the development of portable sensors for food additives.

  3. Extraction as a source of additional information when concentrations in multicomponent systems are simultaneously determined

    International Nuclear Information System (INIS)

    Perkov, I.G.

    1988-01-01

    Using as an example photometric determination of Nd and Sm in their joint presence, the possibility to use the influence of extraction on analytic signal increase is considered. It is shown that interligand exchange in extracts in combination with simultaneous determination of concentrations can be used as a simple means increasing the accuracy of determination. 5 refs.; 2 figs.; 3 tabs

  4. Simultaneous Determination of 6-Mercaptopurine and its Oxidative Metabolites in Synthetic Solutions and Human Plasma using Spectrophotometric Multivariate Calibration Methods

    Directory of Open Access Journals (Sweden)

    Mohammad-Reza Rashidi

    2011-06-01

    Full Text Available Introduction: 6-Mercaptopurine (6MP is an important chemotherapeutic drug in the conventional treatment of childhood acute lymphoblastic leukemia (ALL. It is catabolized to 6-thiouric acid (6TUA through 8-hydroxo-6-mercaptopurine (8OH6MP or 6-thioxanthine (6TX intermediates. Methods: High-performance liquid chromatography (HPLC is usually used to determine the contents of therapeutic drugs, metabolites and other important biomedical analytes in biological samples. In the present study, the multivariate calibration methods, partial least squares (PLS-1 and principle component regression (PCR have been developed and validated for the simultaneous determination of 6MP and its oxidative metabolites (6TUA, 8OH6MP and 6TX without analyte separation in spiked human plasma. Mixtures of 6MP, 8-8OH6MP, 6TX and 6TUA have been resolved by PLS-1 and PCR to their UV spectra. Results: Recoveries (% obtained for 6MP, 8-8OH6MP, 6TX and 6TUA were 94.5-97.5, 96.6-103.3, 95.1-96.9 and 93.4-95.8, respectively, using PLS-1 and 96.7-101.3, 96.2-98.8, 95.8-103.3 and 94.3-106.1, respectively, using PCR. The NAS (Net analyte signal concept was used to calculate multivariate analytical figures of merit such as limit of detection (LOD, selectivity and sensitivity. The limit of detections for 6MP, 8-8OH6MP, 6TX and 6TUA were calculated to be 0.734, 0.439, 0.797 and 0.482 µmol L-1, respectively, using PLS and 0.724, 0.418, 0783 and 0.535 µmol L-1, respectively, using PCR. HPLC was also applied as a validation method for simultaneous determination of these thiopurines in the synthetic solutions and human plasma. Conclusion: Combination of spectroscopic techniques and chemometric methods (PLS and PCR has provided a simple but powerful method for simultaneous analysis of multicomponent mixtures.

  5. Simultaneous spectrophotometric determination of copper, cobalt, nickel and iron in foodstuffs and vegetables with a new bis thiosemicarbazone ligand using chemometric approaches.

    Science.gov (United States)

    Rohani Moghadam, Masoud; Poorakbarian Jahromi, Sayedeh Maria; Darehkordi, Ali

    2016-02-01

    A newly synthesized bis thiosemicarbazone ligand, (2Z,2'Z)-2,2'-((4S,5R)-4,5,6-trihydroxyhexane-1,2-diylidene)bis(N-phenylhydrazinecarbothioamide), was used to make a complex with Cu(2+), Ni(2+), Co(2+) and Fe(3+) for their simultaneous spectrophotometric determination using chemometric methods. By Job's method, the ratio of metal to ligand in Ni(2+) was found to be 1:2, whereas it was 1:4 for the others. The effect of pH on the sensitivity and selectivity of the formed complexes was studied according to the net analyte signal (NAS). Under optimum conditions, the calibration graphs were linear in the ranges of 0.10-3.83, 0.20-3.83, 0.23-5.23 and 0.32-8.12 mg L(-1) with the detection limits of 2, 3, 4 and 10 μg L(-1) for Cu(2+), Co(2+), Ni(2+) and Fe(3+) respectively. The OSC-PLS1 for Cu(2+) and Ni(2+), the PLS1 for Co(2+) and the PC-FFANN for Fe(3+) were selected as the best models. The selected models were successfully applied for the simultaneous determination of elements in some foodstuffs and vegetables. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. Simultaneous determination of the content of serotonin, dopamine, noradrenaline and adrenaline in pancreatic islets isolated from fed and starved mice

    International Nuclear Information System (INIS)

    Hansen, S.E.; Hedeskov, C.J.

    1977-01-01

    A highly sensitive double isotope method for the simultaneous determination of serotonin, dopamine, noradrenaline and adrenaline has been developed. Advantages and limitations of the method are discussed. The mentioned biogenic amines are all present in isolated pancreatic islet tissue from albino mice in concentrations ranging from approximately 5-30 μmol per kg wet weight (0.8-5 x 10 -3 pmol/ng DNA). A somewhat higher content of these amines, especially dopamine, was found in pancreatic acinar tissue. The hypothesis that the impaired glucose-induced insulin secretion during starvation partly is caused by an increased content of biogenic amines in the pancreatic islets was not supported by our experiments which showed an unchanged islet content of these amines after 48 h starvation. (author)

  7. Simultaneous determination of the content of serotonin, dopamine, noradrenaline and adrenaline in pancreatic islets isolated from fed and starved mice

    Energy Technology Data Exchange (ETDEWEB)

    Hansen, S E; Hedeskov, C J [Copenhagen Univ. (Denmark)

    1977-01-01

    A highly sensitive double isotope method for the simultaneous determination of serotonin, dopamine, noradrenaline and adrenaline has been developed. Advantages and limitations of the method are discussed. The mentioned biogenic amines are all present in isolated pancreatic islet tissue from albino mice in concentrations ranging from approximately 5-30 ..mu..mol per kg wet weight (0.8-5 x 10/sup -3/ pmol/ng DNA). A somewhat higher content of these amines, especially dopamine, was found in pancreatic acinar tissue. The hypothesis that the impaired glucose-induced insulin secretion during starvation partly is caused by an increased content of biogenic amines in the pancreatic islets was not supported by our experiments which showed an unchanged islet content of these amines after 48 h starvation.

  8. Simultaneous determination of sulfamethoxazole and trimethoprim residues on manufacturing equipment surfaces

    OpenAIRE

    Coutinho, Roberto C.; Barbosa, Elder T.; Sena, Marcelo M.; Pérez, Caridad Noda

    2009-01-01

    A cleaning validation method was developed and validated, based on swabbing sampling and simultaneous chromatographic determination of sulfamethoxazole (SMX) and trimethoprim (TMP) residues. The method presented limits of detection of 0.06 mg mL-1 for SMX and 0.09 mg mL-1 for TMP. It was considered selective, precise, accurate and robust according to the guidelines from ANVISA, the Brazilian regulatory agency, and International Conference on Harmonization. Mean swab recovery factors of 98.5% ...

  9. Process monitored spectrophotometric titration coupled with chemometrics for simultaneous determination of mixtures of weak acids.

    Science.gov (United States)

    Liao, Lifu; Yang, Jing; Yuan, Jintao

    2007-05-15

    A new spectrophotometric titration method coupled with chemometrics for the simultaneous determination of mixtures of weak acids has been developed. In this method, the titrant is a mixture of sodium hydroxide and an acid-base indicator, and the indicator is used to monitor the titration process. In a process of titration, both the added volume of titrant and the solution acidity at each titration point can be obtained simultaneously from an absorption spectrum by least square algorithm, and then the concentration of each component in the mixture can be obtained from the titration curves by principal component regression. The method only needs the information of absorbance spectra to obtain the analytical results, and is free of volumetric measurements. The analyses are independent of titration end point and do not need the accurate values of dissociation constants of the indicator and the acids. The method has been applied to the simultaneous determination of the mixtures of benzoic acid and salicylic acid, and the mixtures of phenol, o-chlorophenol and p-chlorophenol with satisfactory results.

  10. Simultaneous determination of rifampicin, isoniazid and pyrazinamide in tablet preparations by multivariate spectrophotometric calibration.

    Science.gov (United States)

    Goicoechea, H C; Olivieri, A C

    1999-08-01

    The use of multivariate spectrophotometric calibration is presented for the simultaneous determination of the active components of tablets used in the treatment of pulmonary tuberculosis. The resolution of ternary mixtures of rifampicin, isoniazid and pyrazinamide has been accomplished by using partial least squares (PLS-1) regression analysis. Although the components show an important degree of spectral overlap, they have been simultaneously determined with high accuracy and precision, rapidly and with no need of nonaqueous solvents for dissolving the samples. No interference has been observed from the tablet excipients. A comparison is presented with the related multivariate method of classical least squares (CLS) analysis, which is shown to yield less reliable results due to the severe spectral overlap among the studied compounds. This is highlighted in the case of isoniazid, due to the small absorbances measured for this component.

  11. Simultaneous Mass Determination for Gravitationally Coupled Asteroids

    Energy Technology Data Exchange (ETDEWEB)

    Baer, James [Private address, 3210 Apache Road, Pittsburgh, PA 15241 (United States); Chesley, Steven R., E-mail: jimbaer1@earthlink.net [Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, Pasadena, CA 91109 (United States)

    2017-08-01

    The conventional least-squares asteroid mass determination algorithm allows us to solve for the mass of a large subject asteroid that is perturbing the trajectory of a smaller test asteroid. However, this algorithm is necessarily a first approximation, ignoring the possibility that the subject asteroid may itself be perturbed by the test asteroid, or that the encounter’s precise geometry may be entangled with encounters involving other asteroids. After reviewing the conventional algorithm, we use it to calculate the masses of 30 main-belt asteroids. Compared to our previous results, we find new mass estimates for eight asteroids (11 Parthenope, 27 Euterpe, 51 Neimausa, 76 Freia, 121 Hermione, 324 Bamberga, 476 Hedwig, and 532 Herculina) and significantly more precise estimates for six others (2 Pallas, 3 Juno, 4 Vesta, 9 Metis, 16 Psyche, and 88 Thisbe). However, we also find that the conventional algorithm yields questionable results in several gravitationally coupled cases. To address such cases, we describe a new algorithm that allows the epoch state vectors of the subject asteroids to be included as solve-for parameters, allowing for the simultaneous solution of the masses and epoch state vectors of multiple subject and test asteroids. We then apply this algorithm to the same 30 main-belt asteroids and conclude that mass determinations resulting from current and future high-precision astrometric sources (such as Gaia ) should conduct a thorough search for possible gravitational couplings and account for their effects.

  12. Simultaneous Mass Determination for Gravitationally Coupled Asteroids

    Science.gov (United States)

    Baer, James; Chesley, Steven R.

    2017-08-01

    The conventional least-squares asteroid mass determination algorithm allows us to solve for the mass of a large subject asteroid that is perturbing the trajectory of a smaller test asteroid. However, this algorithm is necessarily a first approximation, ignoring the possibility that the subject asteroid may itself be perturbed by the test asteroid, or that the encounter’s precise geometry may be entangled with encounters involving other asteroids. After reviewing the conventional algorithm, we use it to calculate the masses of 30 main-belt asteroids. Compared to our previous results, we find new mass estimates for eight asteroids (11 Parthenope, 27 Euterpe, 51 Neimausa, 76 Freia, 121 Hermione, 324 Bamberga, 476 Hedwig, and 532 Herculina) and significantly more precise estimates for six others (2 Pallas, 3 Juno, 4 Vesta, 9 Metis, 16 Psyche, and 88 Thisbe). However, we also find that the conventional algorithm yields questionable results in several gravitationally coupled cases. To address such cases, we describe a new algorithm that allows the epoch state vectors of the subject asteroids to be included as solve-for parameters, allowing for the simultaneous solution of the masses and epoch state vectors of multiple subject and test asteroids. We then apply this algorithm to the same 30 main-belt asteroids and conclude that mass determinations resulting from current and future high-precision astrometric sources (such as Gaia) should conduct a thorough search for possible gravitational couplings and account for their effects.

  13. Simultaneous Mass Determination for Gravitationally Coupled Asteroids

    International Nuclear Information System (INIS)

    Baer, James; Chesley, Steven R.

    2017-01-01

    The conventional least-squares asteroid mass determination algorithm allows us to solve for the mass of a large subject asteroid that is perturbing the trajectory of a smaller test asteroid. However, this algorithm is necessarily a first approximation, ignoring the possibility that the subject asteroid may itself be perturbed by the test asteroid, or that the encounter’s precise geometry may be entangled with encounters involving other asteroids. After reviewing the conventional algorithm, we use it to calculate the masses of 30 main-belt asteroids. Compared to our previous results, we find new mass estimates for eight asteroids (11 Parthenope, 27 Euterpe, 51 Neimausa, 76 Freia, 121 Hermione, 324 Bamberga, 476 Hedwig, and 532 Herculina) and significantly more precise estimates for six others (2 Pallas, 3 Juno, 4 Vesta, 9 Metis, 16 Psyche, and 88 Thisbe). However, we also find that the conventional algorithm yields questionable results in several gravitationally coupled cases. To address such cases, we describe a new algorithm that allows the epoch state vectors of the subject asteroids to be included as solve-for parameters, allowing for the simultaneous solution of the masses and epoch state vectors of multiple subject and test asteroids. We then apply this algorithm to the same 30 main-belt asteroids and conclude that mass determinations resulting from current and future high-precision astrometric sources (such as Gaia ) should conduct a thorough search for possible gravitational couplings and account for their effects.

  14. Preconcentration NAA for simultaneous multielemental determination in water sample

    International Nuclear Information System (INIS)

    Chatt, A.

    1999-01-01

    Full text: Environment concerns with water, air, land and their interrelationship viz., human beings, fauna and flora. One of the important environmental compartments is water. Elements present in water might face a whole lot of physico-chemical conditions. This poses challenges to measure their total concentrations as well as different species. Preconcentration of the elements present in water samples is a necessary requisites in water analysis. For multi elements concentration measurements, Neutron Activation Analysis (NAA) is one of the preferred analytical techniques due to its sensitivity and selectivity. In this talk preconcentration NAA for multielemental determination in water sample determination will be discussed

  15. Mercury-free simultaneous determination of cadmium and lead at a glassy carbon electrode modified with multi-wall carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Wu Kangbing; Hu Shengshui; Fei Junjie; Bai Wen

    2003-08-18

    A multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE) was described for the simultaneous determination of trace levels of cadmium and lead by anodic stripping voltammetry (ASV). In pH 4.5 NaAc-HAc buffer containing 0.02 mol/l KI, Cd{sup 2+} and Pb{sup 2+} first adsorb onto the surface of a MWNT film coated GCE and then reduce at -1.20 V. During the positive potential sweep, reduced cadmium and lead were oxidized, and two well-defined stripping peaks appeared at -0.88 and -0.62 V. Compared with a bare GCE, a MWNT film coated GCE greatly improves the sensitivity of determining cadmium and lead. Low concentration of I{sup -} significantly enhances the stripping peak currents since it induces Cd{sup 2+} and Pb{sup 2+} to adsorb at the electrode surface. The striping peak currents change linearly with the concentration of Cd{sup 2+} from 2.5x10{sup -8} to 1x10{sup -5} mol/l and with that of Pb{sup 2+} from 2x10{sup -8} to 1x10{sup -5} mol/l. The lowest detectable concentrations of Cd{sup 2+} and Pb{sup 2+} are estimated to be 6x10{sup -9} and 4x10{sup -9} mol/l, respectively. The high sensitivity, selectivity, and stability of this MWNT film coated electrode demonstrated its practical application for a simple, rapid and economical determination of trace levels of Cd{sup 2+} and Pb{sup 2+} in water samples.

  16. Nanomolar simultaneous determination of levodopa and serotonin at a novel carbon ionic liquid electrode modified with Co(OH)2 nanoparticles and multi-walled carbon nanotubes

    International Nuclear Information System (INIS)

    Babaei, Ali; Taheri, Ali Reza; Aminikhah, Majid

    2013-01-01

    Highlights: ► A novel modified carbon ionic liquid electrode is fabricated as Nafion/Co(OH) 2 –MWCNTs/CILE. ► The modified electrode was used as the new sensor for nanomolar simultaneous determinations of L-dopa and serotonin. ► The electrode was impermeable to uric acid and ascorbic acid and other anionic species as electroactive coexistent compounds. ► Several techniques as cyclic voltammetry, differential pulse voltammetry and chronoamperometry were used for investigations. ► The proposed sensor showed a wide linear range, low detection limit, high stability and good reproducibility. -- Abstract: A novel modified carbon ionic liquid electrode is prepared as an electrochemical sensor for simultaneous determination of levodopa (L-dopa) and serotonin (5-HT). The experimental results suggest that a carbon ionic liquid electrode modified with multi-walled carbon nanotubes and cobalt hydroxide nanoparticles, and coated with Nafion (Nafion/Co(OH) 2 –MWCNTs/CILE), accelerates the electron transfer reactions of L-dopa and 5-HT. In addition it shows no significant interferences of uric acid and ascorbic acid as electroactive coexistent compounds with L-dopa and 5-HT in biological systems. The fabricated sensor revealed some advantages such as convenient preparation, good stability and high sensitivity toward 5-HT and L-dopa determination. The DPV data showed that the obtained anodic peak currents were linearly dependent on the L-dopa and 5-HT concentrations in the range of 0.25–225 and 0.05–75 μmol L −1 , respectively. The applicability of the modified electrode was demonstrated by simultaneous determination of 5-HT and L-dopa in human serum

  17. Simultaneous determination of inorganic and organic anions by ion chromatography

    International Nuclear Information System (INIS)

    Park, Yang Soon; Joe, Ki Soo; Han, Sun Ho; Park, Soon Dal; Choi, Kwang Soon

    1999-06-01

    Four methods were investigated for the simultaneous determination of several inorganic and organic anions in aqueous solution by ion chromatography. The first is two columns coupled system. The second is the gradient elution system with an anion exchange column. The third is the system with a mixed-mode stationary phase. The fourth is the system with an anion exchange column and the eluant of low conductivity without ion suppressor. The advantages and disadvantages of individual systems were discussed. The suitable methods were proposed for the application to the samples of the nuclear power industry and the environment. (author)

  18. Simultaneous Determination of Black Tea-Derived Catechins and Theaflavins in Tissues of Tea Consuming Animals Using Ultra-Performance Liquid-Chromatography Tandem Mass Spectrometry

    Science.gov (United States)

    Ganguly, Souradipta; G., Taposh Kumar; Mantha, Sudarshan

    2016-01-01

    The bioavailability, tissue distribution and metabolic fate of the major tea polyphenols, catechins and theaflavins as well as their gallated derivatives are yet to be precisely elucidated on a single identification platform for assessment of their relative bioefficacy in vivo. This is primarily due to the lack of suitable analytical tools for their simultaneous determination especially in an in vivo setting, which continues to constrain the evaluation of their relative health beneficiary potential and therefore prospective therapeutic application. Herein, we report a rapid and sensitive Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-MS/MS) based method for the simultaneous determination of the major catechins and theaflavins in black tea infusions as well as in different vital tissues and body fluids of tea-consuming guinea pigs. This method allowed efficient separation of all polyphenols within seven minutes of chromatographic run and had a lower limit of quantification (LLOQ) of ~5 ng/ml. Using this method, almost all bioactive catechins and theaflavins could be simultaneously detected in the plasma of guinea pigs orally administered 5% black tea for 14 days. Our method could further detect the majority of these polyphenols in the lung and kidney as well as identify the major catechin metabolites in the urine of the tea-consuming animals. Overall, our study presents a novel tool for simultaneous detection and quantitation of both catechins and theaflavins in a single detection platform that could potentially enable precise elucidation of their relative bioavailability and bioefficacy as well as true health beneficiary potential in vivo. Such information would ultimately facilitate the accurate designing of therapeutic strategies utilizing high efficacy formulations of tea polyphenols for effective mitigation of oxidative damage and inflammation in humans as well as prevention of associated diseases. PMID:27695123

  19. Electrochemical fabrication of a novel ZnO/cysteic acid nanocomposite modified electrode and its application to simultaneous determination of sunset yellow and tartrazine.

    Science.gov (United States)

    Dorraji, Parisa S; Jalali, Fahimeh

    2017-07-15

    A new nanocomposite (ZnO/Cysteic acid) was deposited on glassy carbon electrode by cyclic voltammetry. Uniform deposition of the nanocomposite was observed by scanning electron microscopy. The electron transfer characteristics of two food additives, sunset yellow and tartrazine, were greatly improved on the modified electrode. The prepared electrode was used in the sensitive simultaneous determination of sunset yellow and tartrazine by differential pulse voltammetry. Linear calibration curves were obtained in the concentration ranges of 0.1-3.0, and 0.07-1.86μM, and detection limits of 0.03 and 0.01μM for sunset yellow and tartrazine, respectively. The proposed method was evaluated by determination of the dyes in processed soft drinks with satisfactory results (recovery>95% and RSD%<5%). Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Simultaneous determination of ochratoxin A, mycophenolic acid and fumonisin B-2 in meat products

    DEFF Research Database (Denmark)

    Sørensen, Louise Marie; Mogensen, Jesper; Nielsen, Kristian Fog

    2010-01-01

    Here we present a method for simultaneous determination of the fungal metabolites mycophenolic acid, ochratoxin A (OTA) and fumonisin B-2 (FB2) in meat products. Extraction was performed with water-acetonitrile, followed by acetone-induced precipitation of salts and proteins. Purification...

  1. Spectrometer system using a modular echelle spectrograph and a laser-driven continuum source for simultaneous multi-element determination by graphite furnace absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Geisler, Sebastian; Okruss, Michael; Becker-Ross, Helmut; Huang, Mao Dong, E-mail: huang@isas.de; Esser, Norbert; Florek, Stefan

    2015-05-01

    A multi-element absorption spectrometer system has been developed based on a laser-driven xenon continuum source and a modular simultaneous echelle spectrograph (MOSES), which is characterized by a minimized number of optical components resulting in high optical throughput, high transmittance and high image quality. The main feature of the new optical design is the multifunction usage of a Littrow prism, which is attached on a rotation stage. It operates as an order-sorter for the echelle grating in a double-pass mode, as a fine positioning device moving the echelle spectrum on the detector, and as a forwarder to address different optical components, e.g., echelle gratings, in the setup. Using different prisms, which are mounted back to back on the rotation stage, a multitude of different spectroscopic modes like broad-range panorama observations, specific UV–VIS and NIR studies or high resolution zoom investigations of variable spectral channels can be realized. In the UV panorama mode applied in this work, MOSES has simultaneously detectable wavelength coverage from 193 nm to 390 nm with a spectral resolution λ/Δλ of 55,000 (3-pixel criterion). In the zoom mode the latter can be further increased by a factor of about two for a selectable section of the full wavelength range. The applicability and the analytical performance of the system were tested by simultaneous element determination in a graphite furnace, using eight different elements. Compared to an instrument operating in the optimized single line mode, the achieved analytical sensitivity using the panorama mode was typically a factor of two lower. Using the zoom mode for selected elements, comparable sensitivities were obtained. The results confirm the influence of the different spectral resolutions. - Highlights: • Echelle spectrometer with a full frame CCD array detector • High and variable spectral resolution from λ/Δλ of 55,000 to 95,000 • Laser-driven continuum light source

  2. Simultaneous determination of Magnolol and Honokiol by amino acid ionic liquid synchronous fluorescence spectrometry

    Science.gov (United States)

    Liu, Wei; Zhu, Xiashi

    2018-05-01

    A novel method based on amino acid ionic liquids (AAILs) as an additive synchronous fluorescence spectrometry is proposed for simultaneous determination of magnolol (MN) and honokiol (HN) in traditional Chinese medicine Houpu. The overlapping fluorescence spectrum of MN and HN could be completely separated in the AAILs medium. Experiment parameters (the type and concentration of AAILs, pH values and temperature) were discussed. The detection limits of MN and HN reached 1.46 ng/mL, 0.92 ng/mL and the recovery rates ranged from 98.6%-100.7%, 99.7%-100.6%, respectively. This methods was successfully employed for simultaneously determination of MN and HN in real samples. No significant differences could be found in the results of this method and the pharmacopoeia of People's Republic of China 2015 (Ch.P.2015). The experiment mechanisms were discussed by the Gaussian simulation and fluorescence quantum yield.

  3. Simultaneous determination of hydroquinone and catechol at gold nanoparticles mesoporous silica modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Tashkhourian, J., E-mail: tashkhourian@susc.ac.ir [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Daneshi, M.; Nami-Ana, F. [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Behbahani, M.; Bagheri, A. [Department of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran (Iran, Islamic Republic of)

    2016-11-15

    Highlights: • An electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode was developed. • The electrode provides an accessible surface for simultaneous determination of hydroquinone and catechol. • Hydroquinone and catechol are highly toxic to both environment and human even at very low concentrations. - Abstract: A new electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode (AuNPs-MPS) was developed for simultaneous determination of hydroquinone and catechol. Morphology and structure of the AuNPs-MPS were characterized by transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The electrochemical behavior of hydroquinone and catechol were investigated using square wave voltammetry and the results indicate that the electrochemical responses are improved significantly at the modified electrode. The observed oxidative peaks separation of about 120 mV made possible the simultaneous determination of hydroquinone and catechol in their binary-mixture. Under the optimized condition, a linear dynamic range of 10.0 μM–1.0 mM range for hydroquinone with the detection limit of 1.2 μM and from 30.0 μM–1.0 mM for catechol with the detection limit of 1.1 μM were obtained. The applicability of the method was demonstrated by the recovery studies of hydroquinone and catechol in spiked tap water samples.

  4. A sensitive whole-cell biosensor for the simultaneous detection of a broad-spectrum of toxic heavy metal ions.

    Science.gov (United States)

    Cerminati, S; Soncini, F C; Checa, S K

    2015-04-07

    Bacterial biosensors are simple, cost-effective and efficient analytical tools for detecting bioavailable heavy metals in the environment. This work presents the design, construction and calibration of a novel whole-cell fluorescent biosensory device that, simultaneously and with high sensitivity, reports the presence of toxic mercury, lead, cadmium and/or gold ions in aqueous samples. This bio-reporter can be easily applied as an immediate alerting tool for detecting the presence of harmful pollutants in drinking water.

  5. Simultaneous determination of actinide and strontium nuclides by extraction chromatography

    International Nuclear Information System (INIS)

    Vajda, N.; Molnar, Zs.

    1999-01-01

    A relatively fast and simple separation procedure has been developed for the simultaneous determination of thorium, uranium, neptunium, plutonium, americium, curium and strontium radionuclides. Most of the isotopes of these elements are long-lived, pure alpha and beta emitters regarded as 'difficult to determine' ones in the literature. Our major goal was to develop a combined procedure capable for the analysis of all these nuclides in the same sample aliquot so that correlations can be revealed without the errors arising due to inhomogeneity of samples when the radionuclides are determined from different sub-samples. The combined procedure has the advantage that sample destruction becomes simpler and faster, too. The chemical procedure consists of co-precipitations for the pre-concentration of groups of chemically similar elements and extraction chromatographic separations for the purification of individual elements. By means of pre-concentration relatively big samples can be treated offering the possibility of low activity measurements that cannot be performed by analysing small sample amounts. Pre-concentration techniques were always chosen in order to improve the selectivity of the following separation steps. (authors)

  6. Noninvasive determination of optical lever sensitivity in atomic force microscopy

    International Nuclear Information System (INIS)

    Higgins, M.J.; Proksch, R.; Sader, J.E.; Polcik, M.; Mc Endoo, S.; Cleveland, J.P.; Jarvis, S.P.

    2006-01-01

    Atomic force microscopes typically require knowledge of the cantilever spring constant and optical lever sensitivity in order to accurately determine the force from the cantilever deflection. In this study, we investigate a technique to calibrate the optical lever sensitivity of rectangular cantilevers that does not require contact to be made with a surface. This noncontact approach utilizes the method of Sader et al. [Rev. Sci. Instrum. 70, 3967 (1999)] to calibrate the spring constant of the cantilever in combination with the equipartition theorem [J. L. Hutter and J. Bechhoefer, Rev. Sci. Instrum. 64, 1868 (1993)] to determine the optical lever sensitivity. A comparison is presented between sensitivity values obtained from conventional static mode force curves and those derived using this noncontact approach for a range of different cantilevers in air and liquid. These measurements indicate that the method offers a quick, alternative approach for the calibration of the optical lever sensitivity

  7. Noninvasive determination of optical lever sensitivity in atomic force microscopy

    Science.gov (United States)

    Higgins, M. J.; Proksch, R.; Sader, J. E.; Polcik, M.; Mc Endoo, S.; Cleveland, J. P.; Jarvis, S. P.

    2006-01-01

    Atomic force microscopes typically require knowledge of the cantilever spring constant and optical lever sensitivity in order to accurately determine the force from the cantilever deflection. In this study, we investigate a technique to calibrate the optical lever sensitivity of rectangular cantilevers that does not require contact to be made with a surface. This noncontact approach utilizes the method of Sader et al. [Rev. Sci. Instrum. 70, 3967 (1999)] to calibrate the spring constant of the cantilever in combination with the equipartition theorem [J. L. Hutter and J. Bechhoefer, Rev. Sci. Instrum. 64, 1868 (1993)] to determine the optical lever sensitivity. A comparison is presented between sensitivity values obtained from conventional static mode force curves and those derived using this noncontact approach for a range of different cantilevers in air and liquid. These measurements indicate that the method offers a quick, alternative approach for the calibration of the optical lever sensitivity.

  8. Development of the extraction method for the simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge.

    Science.gov (United States)

    Zuliani, Tea; Lespes, Gaetane; Milacic, Radmila; Scancar, Janez

    2010-03-15

    The toxicity and bioaccumulation of organotin compounds (OTCs) led to the development of sensitive and selective analytical methods for their determination. In the past much attention was assigned to the study of OTCs in biological samples, water and sediments, coming mostly from marine environment. Little information about OTCs pollution of terrestrial ecosystems is available. In order to optimise the extraction method for simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge five different extractants (tetramethylammonium hydroxide, HCl in methanol, glacial acetic acid, mixture of acetic acid and methanol (3:1), and mixture of acetic acid, methanol and water (1:1:1)), the presence or not of a complexing agent (tropolone), and the use of different modes of extraction (mechanical stirring, microwave and ultrasonic assisted extraction) were tested. Extracted OTCs were derivatised with sodium tetraethylborate and determined by gas chromatography coupled with mass spectrometer. Quantitative extraction of butyl-, phenyl- and octyltin compounds was obtained by the use of glacial acetic acid as extractant and mechanical stirring for 16h or sonication for 30 min. The limits of detection and quantification for OTCs investigated in sewage sludge were in the ng S ng(-1) range. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of shikimic acid, salicylic acid and jasmonic acid in wild and transgenic Nicotiana langsdorffii plants exposed to abiotic stresses.

    Science.gov (United States)

    Scalabrin, Elisa; Radaelli, Marta; Capodaglio, Gabriele

    2016-06-01

    The presence and relative concentration of phytohormones may be regarded as a good indicator of an organism's physiological state. The integration of the rolC gene from Agrobacterium rhizogenes and of the rat glucocorticoid receptor (gr) in Nicotiana langsdorffii Weinmann plants has shown to determine various physiological and metabolic effects. The analysis of wild and transgenic N. langsdorffii plants, exposed to different abiotic stresses (high temperature, water deficit, and high chromium concentrations) was conducted, in order to investigate the metabolic effects of the inserted genes in response to the applied stresses. The development of a new analytical procedure was necessary, in order to assure the simultaneous determination of analytes and to obtain an adequately low limit of quantification. For the first time, a sensitive HPLC-HRMS quantitative method for the simultaneous determination of salicylic acid, jasmonic acid and shikimic acid was developed and validated. The method was applied to 80 plant samples, permitting the evaluation of plant stress responses and highlighting some metabolic mechanisms. Salicylic, jasmonic and shikimic acids proved to be suitable for the comprehension of plant stress responses. Chemical and heat stresses showed to induce the highest changes in plant hormonal status, differently affecting plant response. The potential of each genetic modification toward the applied stresses was marked and particularly the resistance of the gr modified plants was evidenced. This work provides new information in the study of N. langsdorffii and transgenic organisms, which could be useful for the further application of these transgenes. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  10. Simultaneous determination of sulfonamides, tetracyclines and tiamulin in swine wastewater by solid-phase extraction and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Ben, Weiwei; Qiang, Zhimin; Adams, Craig; Zhang, Heqing; Chen, Liping

    2008-08-22

    Little is known about the contamination level of antibiotics in swine wastewater in China. The highly complex matrix of swine wastewater, which generally has a chemical oxygen demand (COD) concentration as high as 15,000 mg/L, makes it difficult to detect antibiotics at trace levels. In this work, a highly selective and sensitive analytical method was developed for simultaneous determination of three classes of commonly used veterinary antibiotics including five sulfonamides, three tetracyclines and one macrolide in swine wastewater using solid-phase extraction (SPE) and liquid chromatography-mass spectrometry (LC-MS). The method detection limits (MDL) in the swine wastewater were determined to be between 5 and 91 ng/L, depending on specific antibiotics. Except sulfamethizole, all the other eight antibiotics were detected in the swine wastewaters collected from three concentrated swine feeding plants located in the Beijing (China) area, showing a concentration range of 0.62-32.67 microg/L. These results reveal the representative concentration levels of selected antibiotics in the swine wastewaters of Beijing area.

  11. Determine Multiple Elements Simultaneously in the Sera of Umbilical Cord Blood Samples-a Very Simple Method.

    Science.gov (United States)

    Liang, Chunmei; Li, Zhijuan; Xia, Xun; Wang, Qunan; Tao, Ruiwen; Tao, Yiran; Xiang, Haiyun; Tong, Shilu; Tao, Fangbiao

    2017-05-01

    Analyzing the concentrations of heavy metals in the sera of umbilical cord blood samples can provide useful information about prenatal exposure to environmental agents. An analytical method based on ICP-MS to simultaneously determine multiple elements in umbilical cord blood samples was developed for assessing the in utero exposure to metallic and metalloid elements. The method only required as little as 100 μL of serum diluted 1:25 for direct analysis. Matrix-matched protocol was used to eliminate mass matrix interference and kinetic energy discrimination mode was used to eliminate the polyatomic ion interference. The assay was completed on average within 4 min with the detection limits ranging from 0.0002 to 44.4 μg/L for all the targeted elements. The detection rates for most of elements were 100 % other than cadmium (Cd), lead (Pb), and mercury (Hg). The testing results of the certified reference materials were ideal. The method is simple and sensitive, so it is suitable for the monitoring of large quantities of samples.

  12. Simultaneous detection of water-soluble vitamins using the High Performance Liquid Chromatography (HPLC - a review

    Directory of Open Access Journals (Sweden)

    Rosemond Godbless Dadzie

    2014-01-01

    Full Text Available The water-soluble vitamins (WSV: ascorbic acid (vitamin C, thiamine (B1, riboflavin (B2, niacin (B3, panthothenic acid (B5, pyridoxine, and pyridoxal (B6, folic acid (B9, biotin(B8 , and B12 are very essential in the diet of humankind. As a result of ever increasing pressures from both consumers and legal enforcers, to specify accurately nutritive compositions of WSV that are present in food materials, many researchers have attempted to fill this niche through the provision of highly sensitive and rapid high performance liquid chromatography (HPLC procedures. In view of the health benefits of WSV, a replete of HPLC methods have been developed for simultaneous determination of their contents in nature and fortified food samples, nutritional supplements, as well as blood plasmas. The rate of losses of these vitamins during food processing and analysis, in addition to their transient dynamics, presents complexities in developing a highly sensitive HPLC procedure for their simultaneous separations and assays. This review critically assesses the different HPLC procedures developed by researchers and available in the open literature for simultaneous determination of water-soluble vitamins (WSV in dried tropical fruits materials. The study revealed that not a single chromatographic run developed by researchers can simultaneously elute all the WSV at a time. However, the HPLC procedures that are capable of determining all the WSV were coupled with electrospray ionization mass spectroscopy (ESI-MS, thus making the set-up expensive.

  13. A universal gamma-gamma method for simultaneous determination of rock and ore properties

    International Nuclear Information System (INIS)

    Charbucinski, J.

    1983-01-01

    A method for the simultaneous determination of heavy element content, density, borehole diameter and grain size is described, which is based on investigation of the changes in spectrum shape. By analysing these changes in a quantitative manner, information regarding the physical parameters of the medium can be obtained. The results of laboratory tests of the method are presented. (author)

  14. An in-line fiber-optic modal interferometer for simultaneous measurement of twist and ambient temperature

    Directory of Open Access Journals (Sweden)

    Yongqin Yu

    2014-12-01

    Full Text Available A novel and simple sensor based on fiber-optic modal interferometer fabricated by a segment of low elliptical hollow-core photonic bandgap fiber for simultaneous temperature and twist measurements is demonstrated. Meanwhile the sensor can also measure the twist angle and determine the twist direction simultaneously. The mode distribution of EHC-PBGF is demonstrated both in theory and experiments. There is an obvious difference of two transmission dips on the temperature and twist. The twist sensitivities of Dip 1 and Dip 2 are obtained to be −31.95 and −585.8 pm/(rad/m, respectively. The temperature sensitivities are 12.99 pm/°C for Dip 1 and 5.09 pm/°C for Dip 2, respectively. Two parameters of twist and temperature can be distinguished and measured simultaneously by using a sensing matrix. Meanwhile the structure is found to be weakly sensitive to the axial strain. It has the advantage of avoiding the crosstalk of strain in the applications.

  15. High-sensitive LC-MS/MS method for the simultaneous determination of mirodenafil and its major metabolite, SK-3541, in human plasma: application to microdose clinical trials of mirodenafil.

    Science.gov (United States)

    Cho, Doo-Yeoun; Bae, Soo Hyeon; Shon, Ji-Hong; Bae, Soo Kyung

    2013-03-01

    A high-sensitivity LC/MS/MS method was developed and validated for the simultaneous determination of mirodenafil and its major metabolite, SK-3541, in human plasma. Mirodenafil, SK-3541, and udenafil as an internal standard were extracted from plasma samples with methyl tert-butyl ether. Chromatographic separation was performed on a Luna phenyl-hexyl column (100 × 2.0 mm) with an isocratic mobile phase consisting of 5 mM ammonium formate and ACN (23:77, v/v) at a flow rate of 0.35 mL/min. Detection and quantification were performed using a mass spectrometer in selected reaction monitoring mode with positive ESI at m/z 532.3 → 296.1 for mirodenafil, m/z 488.1 → 296.1 for SK-3541, and m/z 517.3 → 283.2 for udenafil. The calibration curves were linear over a concentration range of 2-500 pg/mL using 0.5 mL plasma for the microdose of mirodenafil (100 μg). Analytical method validation of the clinical dose (100 mg), with a calibration curve range of 2-500 ng/mL using 0.025-mL plasma, was also conducted. The other LC-MS/MS conditions were similar to those used for the microdosing. Each method was applied successfully to pharmacokinetic studies after a microdose or clinical dose of mirodenafil to six healthy Korean male volunteers. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Simultaneous determination of glycols based on fluorescence anisotropy

    International Nuclear Information System (INIS)

    Garcia Sanchez, F.; Navas Diaz, A.; Lopez Guerrero, M.M.

    2007-01-01

    Simultaneous determination of non-fluorescent glycols in mixtures without separation or chemical transformation steps is described. Two methods based in the measure of fluorescence anisotropy of a probe such as fluorescein dissolved in the analyte or analyte mixtures are described. In the first method, the anisotropy spectra of pure and mixtures of analytes are used to quantitative determination (if the fluorophor concentration is in a range where fluorescence intensity is proportional to concentration). In the second method, a calibration curve anisotropy-concentration based on the application of the Perrin equation is established. The methods presented here are capable of directly resolving binary mixtures of non-fluorescent glycols on the basis of differences on the fluorescence anisotropy of a fluorescence tracer. Best analytical performances were obtained by application of the method based on Perrin equation. This method is simple, rapid and allows the determination of mixtures of glycols with reasonable accuracy and precision. Detection limits are limited by the quantum yield and anisotropy values of the tracer in the solvents. Recovery values are related to the differences in anisotropy values of the tracer in the pure solvents. Mixtures of glycerine/ethylene glycol (GL/EG), ethylene glycol/1,2-propane diol (EG/1,2-PPD) and polyethylene glycol 400/1,2-propane diol (PEG 400/1,2-PPD) were analysed and recovery values are within 95-120% in the Perrin method. Relative standard deviation are in the range 1.3-2.9% and detection limits in the range 3.9-8.9%

  17. Simultaneous determination of aluminium and phosphorus by neutron activation analysis

    International Nuclear Information System (INIS)

    Gatschke, W.; Gawlik, D.

    1980-01-01

    With the use of the pneumatic tube system of the BER II reactor, the irradiation position of which is equipped with a movable cadmium shield, the aluminium and phosphorus levels in bone powder and in human bone biopsies were determined. The contribution of aluminium and phosphorus to the 28 Al activity could be separated mathematically after the samples had been irradiated with and without cadmium shielding. The sensitivity and limit of quantitative determination of the analytical procedure were determined using the addition method and the fact that the levels of each element measured was independent of the amount of the other element was proved. (author)

  18. Nanomolar simultaneous determination of tryptophan and melatonin by a new ionic liquid carbon paste electrode modified with SnO{sub 2}-Co{sub 3}O{sub 4}@rGO nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Zeinali, Homa [Department of Chemistry, Payame Noor University, Qazvin (Iran, Islamic Republic of); Bagheri, Hasan, E-mail: h.bagheri82@gmail.com [Chemical Injuries Research Center, Baqiyatallah University of Medical Sciences, Tehran (Iran, Islamic Republic of); Monsef-Khoshhesab, Zahra [Department of Chemistry, Payame Noor University, Qazvin (Iran, Islamic Republic of); Khoshsafar, Hosein [Department of Internal Medicine, Zabol University of Medical Sciences, Zabol (Iran, Islamic Republic of); Hajian, Ali [Laboratory for Sensors, Department of Microsystems Engineering (IMTEK), University of Freiburg, Georges Köhler Allee 103, 79110 Freiburg (Germany)

    2017-02-01

    This work describes the development of a new sensor for simultaneous determination of tryptophan and melatonin. The proposed sensor was an ionic liquid carbon paste electrode modified with reduced graphene oxides decorated with SnO{sub 2}-Co{sub 3}O{sub 4} nanoparticles. The voltammetric oxidation of the analytes by the proposed sensor confirmed that the electrooxidation process undergoes a two-electron/one-proton reaction for melatonin and a two-electron/two-proton reaction for tryptophan in diffusion-controlled processes. Moreover, based on the excellent electrochemical properties of the modified electrode, a sensitive voltammetric method was used for individual and simultaneous determination of melatonin and tryptophan in the aqueous solutions. Under the optimized experimental conditions, a linear response obtained in the range of 0.02 to 6.00 μmol L{sup −1} with detection limits of 4.1 and 3.2 nmol L{sup −1} for melatonin and tryptophan, respectively. The prepared sensor possessed accurate and rapid response toward melatonin and tryptophan with a good sensitivity, selectivity, stability, and repeatability. Finally, the applicability of the proposed sensor was verified by evaluation of melatonin and tryptophan in various real samples including human serum and tablet samples. - Highlights: • Ionic liquid-SnO{sub 2}-Co{sub 3}O{sub 4}@rGO nanocomposite as electrode material • This modifier can promote the electrochemical properties of carbon paste electrode. • Determination of tryptophan and melatonin was investigated.

  19. Simultaneous Determination of Arsenic, Manganese, and Selenium in Biological Materials by Neutron-Activation Analysis

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Damsgaard, Else

    1973-01-01

    A new method was developed for the simultaneous determination of arsenic, manganese, and selenium in biological material by thermal-neutron activation analysis. The use of 81 mSe as indicator for selenium permitted a reduction of activation time to 1 hr for a 1 g sample, and the possibility of loss...

  20. Simultaneous determination of uranium and plutonium in dissolver solution of irradiated fuel, using ID-TIMS. IRP-11

    International Nuclear Information System (INIS)

    Shah, Raju; Sasi Bhushan, K.; Govindan, R.; Alamelu, D.; Khodade, P.S.; Aggarwal, S.K.

    2007-01-01

    A simple sample preparation and simultaneous analysis method to determine uranium and plutonium from dissolver solution, employing the technique of Isotope Dilution Mass spectrometry has been demonstrated. The method used, co-elusion of Uranium and Plutonium from anion exchanger column after initial elution of major part of uranium in 1:5 HNO 3 in order to reduce the initial U/Pu ratio from 1000 to about 100-200 in the co-eluted fraction. Due to the availability of variable multi-collector system, different Faraday cups were adjusted to collect the different ion intensities corresponding to the different masses, during the simultaneous analysis of Uranium and Plutonium, loaded on Re double filament assembly. 233 U and PR grade Plutonium were used as spikes to determine Uranium and Plutonium from dissolver solution of irradiated fuel from research reactor. The possibility of getting the isotopic composition of uranium from the simultaneous analysis of co-eluted purified fraction of U and Pu from spiked aliquots is also explained. (author)

  1. The fractioning factor and the number of theorical plates in isotopic enrichment columns determined simultaneously

    International Nuclear Information System (INIS)

    Ducatti, Carlos

    1997-01-01

    Using an analytical approach and an analytical graphical method, it was determined simultaneously the fractioning factor and the number of theoretical plates in isotopic enrichment columns during the conditions of dinamical isotopic equilibrium. (author). 5 refs., 2 figs., 2 tabs

  2. Chemically sensitive interfaces on SAW devices

    Energy Technology Data Exchange (ETDEWEB)

    Ricco, A.J.; Martin, S.J. [Sandia National Labs., Albuquerque, NM (United States); Crooks, R.M.; Xu, Chuanjing [Texas A and M Univ., College Station, TX (United States); Allred, R.E. [Adherent Technologies, Inc., Albuquerque, NM (United States)

    1993-11-01

    Using surface acoustic wave (SAW) devices, three approaches to the effective use of chemically sensitive interfaces that are not highly chemically selective have been examined: (1) molecular identification from time-resolved permeation transients; (2) using multifrequency SAW devices to determine the frequency dependence of analyte/film interactions; (3) use of an array of SAW devices bearing diverse chemically sensitive interfaces to produce a distinct response pattern for each analyte. In addition to their well-known sensitivity to mass changes (0.0035 monolayer of N{sub 2} can be measured), SAW devices respond to the mechanical and electronic properties of thin films, enhancing response information content but making a thorough understanding of the perturbation critical. Simultaneous measurement of changes in frequency and attenuation, which can provide the information necessary to determine the type of perturbation, are used as part of the above discrimination schemes.

  3. Simultaneous determination of U and Pu isotopes by alpha spectrometry

    International Nuclear Information System (INIS)

    Equillor, H.E.; Campos, J.M.

    2011-01-01

    Determination of actinides by alpha spectrometry is usually carried out after full separation of each of the components of the sample. The procedure presented in this paper permits U and Pu isotopes to be measured together allowing faster sample processing and measurement. The method consists in the extraction with tributyl phosphate of U and Pu isotopes from the rest of the matrix, followed by a cathodic electrodeposition to obtain alpha spectrometry suitable pieces. It can be applied to various environmental samples, such as water, filters and soil (about 0.5 g of solid sample for the described conditions). High-quality electroplated discs are essential for simultaneous processing, so a technique to achieve this requirement is also explained. (authors) [es

  4. Simultaneous determination of metolazone and valsartan in plasma by on-line SPE coupled with liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Jiezhao; Chen, Meiling; Li, Ying; Yu, Fanglin; Cheng, Xiaohui; Yang, Yang; Liu, Yan; Xie, Xiangyang; Li, Zhiping; Zhang, Hui; Mei, Xingguo

    2017-10-01

    Combination of metolazone (0.5 mg) and valsartan (80 mg) has been verified as a promising therapy treatment for hypertension. In order to facilitate to pharmacokinetic research, it needs a method for the simultaneously determination of metolazone and valsartan in biological samples. However, there are no relative reports so far. In order to facilitate to pharmacokinetic research, an on-line solid phase extraction coupled with liquid chromatography-tandem mass spectrometry method for the simultaneous determination of metolazone and valsartan in beagle dog plasma was developed and validated in this study. An on-line solid phase extraction column Retain PEP Javelin (10 mm × 2.1 mm) was used to remove impurities in plasma samples. The metolazone, valsartan and internal standard (losartan) were separated on a Poroshell 120 SB-C18 column (4.6 mm × 50 mm × 2.7 µm) with a gradient elution procedure. Acidified acetonitrile/water mixture was used as a mobile phase. The selected multiple-reaction monitoring mode in positive ion was performed and the parent to the product transitions m/z 366/259, m/z 436.2/291 and m/z 423.4/207 were used to measure the metolazone, valsartan and losartan. The method was linear over the range of 0.1-100 ng/mL and 1-1000 ng/mL for metolazone and valsartan, respectively. This method was validated in terms of specificity, linearity, sensitivity, precision, accuracy, matrix effect, and stability and then successfully applied to pharmacokinetic studies of the metolazone and valsartan combination tablets in beagle dogs.

  5. Simultaneous determination of caffeine, theobromine, and theophylline by high-performance liquid chromatography.

    Science.gov (United States)

    Bispo, Marcia S; Veloso, Márcia Cristina C; Pinheiro, Heloísa Lúcia C; De Oliveira, Rodolfo F S; Reis, José Oscar N; De Andrade, Jailson B

    2002-01-01

    This work relates the development of an analytical methodology to simultaneously determine three methylxanthines (caffeine, theobromine, and theophylline) in beverages and urine samples based on reversed-phase high-performance liquid chromatography. Separation is made with a Bondesil C18 column using methanol-water-acetic acid or ethanol-water-acetic acid (20:75:5, v/v/v) as the mobile phase at 0.7 mL/min. Identification is made by absorbance detection at 273 nm. Under optimized conditions, the detection limit of the HPLC method is 0.1 pg/mL for all three methylxanthines. This method is applied to urine and to 25 different beverage samples, which included coffee, tea, chocolate, and coconut water. The concentration ranges determined in the beverages and urine are: < 0.1 pg/mL to 350 microg/mL and 3.21 microg/mL to 71.2 microg/mL for caffeine; < 0.1 pg/mL to 32 microg mL and < 0.1 pg/mL to 13.2 microg/mL for theobromine; < 0.1 pg/mL to 47 microg/mL and < 0.1 pg/mL to 66.3 microg/mL for theophylline. The method proposed in this study is rapid and suitable for the simultaneous quantitation of methylxanthines in beverages and human urine samples and requires no extraction step or derivatization.

  6. Simultaneous determination of hydroquinone and catechol based on glassy carbon electrode modified with gold-graphene nanocomposite

    International Nuclear Information System (INIS)

    Ma, X.; Liu, Z.; Qiu, C.; Chen, T.; Ma, H.

    2013-01-01

    We have synthesized a virtually monodisperse gold-graphene (Au-G) nanocomposite by a single-step chemical reduction method in aqueous dimethylformamide solution. The nanoparticles are homogenously distributed over graphene nanosheets. A glassy carbon electrode was modified with this nanocomposite and displayed high electrocatalytic activity and extraordinary electronic transport properties due to its large surface area. It enabled the simultaneous determination of hydroquinone (HQ) and catechol (CC) in acetate buffer solution of pH 4.5. Two pairs of well-defined, quasi-reversible redox peaks are obtained, one for HQ and its oxidized form, with a 43 mV separation of peak potentials (ΔEp), the other for CC and its oxidized form, with a ΔEp of 39 mV. Due to the large separation of oxidation peak potentials (102 mV), the concentrations of HQ and CC can be easily determined simultaneously. The oxidation peak currents for both HQ and CC increase linearly with the respective concentrations in the 1.0 μM to 0.1 mM concentration range, with the detection limits of 0.2 and 0. 15 μM (S/N = 3), respectively. The modified electrode was successfully applied to the simultaneous determination of HQ and CC in spiked tap water, demonstrating that the Au-G nanocomposite may act as a high-performance sensing material in the selective detection of some environmental pollutants. (author)

  7. Simultaneous Determination of Mutagenicity and Toxicity of ...

    African Journals Online (AJOL)

    A demonstration of cytotoxicity is required (measurement of cell number, culture confluency and inhibition of mitotic index) for in vitro cytogenetic assays. The study therefore investigated whether delayed cytotoxicity can be used to simultaneously predict mutagenicity and cytotoxicty. Chinese hamster lung cells were ...

  8. Simultaneous determination of isoniazid and pyrazinamide in ...

    African Journals Online (AJOL)

    Finally, 20 µL was injected into the HPLC system. HPLC analysis ... The method was accurate, and relative error ... Keywords: HPLC, Isoniazid, Pyrazinamide, Plasma, Simultaneous analysis. Tropical ... work, we describe a new HPLC method with UV ... pooled human plasma. ..... License, which permits unrestricted use,.

  9. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

  10. Simultaneous determination of borate, chloride and molybdate in pyrohydrolysis distillates of plant and soil samples by ion chromatography.

    Science.gov (United States)

    Mishra, Vivekchandra Guruprasad; Das, Mrinal Kanti; Shah, Dipti Jayesh; Jeyakumar, Subbiah; Tomar, Bhupendra Singh; Ramakumar, Karanam Lakshminarayana

    2018-01-12

    Determination of concentrations of micronutrients in plant samples is important in order to assess the growth and quality of plants. An ion chromatography (IC) method was developed for the simultaneous determination of B, Cl and Mo (micronutrients present in their anionic form in aqueous samples) using a gradient elution with d-mannitol and NaOH. Despite their different chemical nature, these elements could be separated from the matrix by employing pyrohydrolysis. IC was employed for their sequential determination from single aliquot injection into the IC column. It was observed that the optimised procedures developed earlier in our laboratory for the separation of B and halogens using d-Mannitol-NaOH or bicarbonate eluents could not be extended to B-Mo-Cl separation. The concentration levels of d-mannitol in the eluent required for separation of boron impeded the conductivity detection of Mo and the peak sensitivity was seen to be critically dependent on d-mannitol concentration in the eluent. In addition, d-mannitol in NaOH eluent altered the retention times of analytes (B, F - , Cl - , NO 3 - , SO 4 2- and MoO 4 2- ) which were not observed in the case of bicarbonate eluent. The current study deals with the investigation on the influence of d-mannitol on the molybdate as well as its role on the retention time. Formation of Mo-mannitol complex at different pH conditions and de-protonation of mannitol were correlated to the observed effects. Based on the observations, a gradient elution method was proposed for the simultaneous separation and determination of B, Cl and Mo in the pyrohydrolysis distillates of plant samples. The method was calibrated for B (0.05-1 mg/L), Cl (0.1-10 mg/L) and Mo (0.5-10 mg/L) and the linear regression coefficients obtained were 0.9992, 0.9998 and 0.997 respectively. The limit of detection (LOD) for B, Cl and Mo was calculated to be 19, 23 and 96 μg/L, respectively. The developed IC method after pyrohydrolytic separation of B

  11. Simultaneous Determination of Ciprofloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Eye Drops by HPLC

    Directory of Open Access Journals (Sweden)

    Prakash Katakam

    2012-01-01

    Full Text Available A liquid chromatographic method was developed and validated for the simultaneous determination of ciprofloxacin hydrochloride and dexamethasone sodium phosphate in bulk and pharmaceutical formulations. Optimum separation was achieved in less than 5 min using a C18 column (250 mmx4.6 mm i.d, 5μ particle size by isocratic elution. The mobile phase consisting of a mixture of mixed phosphate buffer (pH 4 and acetonitrile (65:35, v/v was used. Column effluents were monitored at 254 nm at a flow rate of 1ml/min. Retention times of ciprofloxacin hydrochloride and dexamethasone sodium phosphate were 2.0 and 3.16 min respectively. The linearity of ciprofloxacin hydrochloride and dexamethasone sodium phosphate was in the range of 3-18 μg/ml and 1-6 μg/ml respectively. Developed method was economical in terms of the time taken and amount of solvent consumed for each analysis. The method was validated and successfully applied to the simultaneous determination of ciprofloxacin hydrochloride and dexamethasone sodium phosphate in bulk and pharmaceutical formulations.

  12. Simultaneous multi-element atomic absorption system using photodiode array detector

    International Nuclear Information System (INIS)

    Tong, S.L.; Chin, K.S.

    1994-01-01

    A photodiode array (PDA) detector-multichannel analyser (MCA) system has been coupled to a flame and a graphite furnace atomiser and tested for simultaneous multielement atomic absorption analysis. Multielement hollow cathode lamps (HCL) are used as light source. Spectral lines are dispersed through a spectrograph with triple gratings and detected by a 25.4 mm PDA detector consisting of 1024 elements. The optical MCA system is capable of recording multiple spectra spanned by the spectrograph/PDA. The transmitted intensity spectra obtained for the standard and analyte solutions during flame or graphite furnace atomisation are converted to absorbance spectra using the MCA software provided. Results from the comparison studies show that the linear range and sensitivities for Ni-Co-Fe and Cu-Cr obtained from the simultaneous measurements are within the same order of magnitudes as those from conventional single element determinations using photomultiplier tube detection. The study also shows that non-atomic absorption can be readily corrected by a two-line method where non-atomic absorption lines can be chosen from the spectra recorded simultaneously. The proposed system has been evaluated for the determination of trace elements using NBS standard reference water SRM 1643b

  13. Application of different spectrophotometric methods for simultaneous determination of elbasvir and grazoprevir in pharmaceutical preparation

    Science.gov (United States)

    Attia, Khalid A. M.; El-Abasawi, Nasr M.; El-Olemy, Ahmed; Abdelazim, Ahmed H.

    2018-01-01

    The first three UV spectrophotometric methods have been developed of simultaneous determination of two new FDA approved drugs namely; elbasvir and grazoprevir in their combined pharmaceutical dosage form. These methods include simultaneous equation, partial least squares with and without variable selection procedure (genetic algorithm). For simultaneous equation method, the absorbance values at 369 (λmax of elbasvir) and 253 nm (λmax of grazoprevir) have been selected for the formation of two simultaneous equations required for the mathematical processing and quantitative analysis of the studied drugs. Alternatively, the partial least squares with and without variable selection procedure (genetic algorithm) have been applied in the spectra analysis because the synchronous inclusion of many unreal wavelengths rather than by using a single or dual wavelength which greatly increases the precision and predictive ability of the methods. Successfully assay of the drugs in their pharmaceutical formulation has been done by the proposed methods. Statistically comparative analysis for the obtained results with the manufacturing methods has been performed. It is noteworthy to mention that there was no significant difference between the proposed methods and the manufacturing one with respect to the validation parameters.

  14. Simultaneous Determination of Eosin-Yellow and Ponceau-S Using H-Point Standard Addition Method in Micellar Media

    Directory of Open Access Journals (Sweden)

    Amandeep Kaur

    2012-01-01

    Full Text Available H-point standard addition method (HPSAM is developed for simultaneous determination of eosin-Y and ponceau-s in micellar media. Nickel chloride (NiCl2 is used as chromogenic reagent for complexes formation of eosin-Y and ponceau-S food colorants. The measurements were carried out using sodium lauryl sulphate as a surfactant, in buffered solution at pH 6.0. The concentration range of 0.115-2.53 μg/mL of eosin-Y and 0.159-3.80 μg/mL of ponceau-S. The proposed procedures have been applied successfully for the simultaneous determination of eosin-Y and ponceau-S in synthetic binary mixtures and real samples.

  15. Fractionation of human serum lipoproteins and simultaneous enzymatic determination of cholesterol and triglycerides

    International Nuclear Information System (INIS)

    Qureshi, Rashid Nazir; Kok, Wim Th.; Schoenmakers, Peter J.

    2009-01-01

    A method based on Asymmetric Flow Field-Flow Fractionation (AF4) was developed to separate different types of lipoproteins from human serum. The emphasis in the method optimization was on the possibilities to characterize the largest lipoprotein fractions (LDL and VLDL), which is usually not possible with the size-exclusion chromatography methods applied in routine analysis. Different channel geometries and flow programs were tested and compared. The use of a short fractionation channel was shown to give less sample dilution at the same fractionation power compared to a conventional, long channel. Different size selectivities were obtained with an exponential decay and a linear cross flow program. The ratio of the UV absorption signal to the light scattering signal was used to validate the relation between retention time and size of the fractionated particles. An experimental setup was developed for the simultaneous determination of the cholesterol and triglycerides distribution over the lipoprotein fractions, based on enzymatic reactions followed by UV detection at 500 nm. Coiled and knitted PTFE tubing reactors were compared. An improved peak sharpness and sensitivity were observed with the knitted tubing reactor. After optimization of the experimental conditions a satisfactory linearity and precision (2-3% rsd for cholesterol and 5-6% rsd for triglycerides) were obtained. Finally, serum samples, a pooled sample from healthy volunteers and samples of sepsis patients, were analyzed with the method developed. Lipoprotein fractionation and cholesterol and triglyceride distributions could be correlated with the clinical background of the samples.

  16. Fractionation of human serum lipoproteins and simultaneous enzymatic determination of cholesterol and triglycerides

    Energy Technology Data Exchange (ETDEWEB)

    Qureshi, Rashid Nazir [Polymer-Analysis Group, van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam (Netherlands); Kok, Wim Th., E-mail: W.Th.Kok@uva.nl [Polymer-Analysis Group, van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam (Netherlands); Schoenmakers, Peter J. [Polymer-Analysis Group, van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam (Netherlands)

    2009-11-03

    A method based on Asymmetric Flow Field-Flow Fractionation (AF4) was developed to separate different types of lipoproteins from human serum. The emphasis in the method optimization was on the possibilities to characterize the largest lipoprotein fractions (LDL and VLDL), which is usually not possible with the size-exclusion chromatography methods applied in routine analysis. Different channel geometries and flow programs were tested and compared. The use of a short fractionation channel was shown to give less sample dilution at the same fractionation power compared to a conventional, long channel. Different size selectivities were obtained with an exponential decay and a linear cross flow program. The ratio of the UV absorption signal to the light scattering signal was used to validate the relation between retention time and size of the fractionated particles. An experimental setup was developed for the simultaneous determination of the cholesterol and triglycerides distribution over the lipoprotein fractions, based on enzymatic reactions followed by UV detection at 500 nm. Coiled and knitted PTFE tubing reactors were compared. An improved peak sharpness and sensitivity were observed with the knitted tubing reactor. After optimization of the experimental conditions a satisfactory linearity and precision (2-3% rsd for cholesterol and 5-6% rsd for triglycerides) were obtained. Finally, serum samples, a pooled sample from healthy volunteers and samples of sepsis patients, were analyzed with the method developed. Lipoprotein fractionation and cholesterol and triglyceride distributions could be correlated with the clinical background of the samples.

  17. Simultaneous determination of cucurbitacin B, E, I and E-glucoside in plant material and body fluids by HPLC-MS.

    Science.gov (United States)

    Bajcsik, Nicole; Pfab, Rudolf; Pietsch, Jörg

    2017-05-01

    A selective and sensitive analytical method for the simultaneous determination of cucurbitacin B, E, I and E-glucoside in plant material and body fluids by HPLC-MS was developed. After liquid-liquid extraction with dichlormethane, separation was achieved on a Phenomenex Luna Pentafluorophenyl Column (150mm×2mm, 5μm) using acetonitrile-water (90:10, v/v) as mobile phase system. Detection was performed using a 3200 Q Trap mass spectrometer (AB Sciex). For analysis Q1 Scans with negative ionisation were chosen. The method was validated for serum as the matrix of choice. Limits of detection are in the picogram range, limits of quantification are between 0.05 and 0.42ng/mL, recoveries are above 50%. The assay was linear in the calibration range from 1.0 to 50ng/mL for cucurbitacin E and from 0.10 to 50ng/mL for the cucurbitacins B, I and E-glucoside. The applicability of the method was demonstrated by the determination of cucurbitacins in zucchini plant material and body fluids from intoxication cases. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Determination of Chlorinated Hydrocarbons in Water Using Highly Sensitive Mid-Infrared Sensor Technology

    Science.gov (United States)

    Lu, Rui; Mizaikoff, Boris; Li, Wen-Wei; Qian, Chen; Katzir, Abraham; Raichlin, Yosef; Sheng, Guo-Ping; Yu, Han-Qing

    2013-08-01

    Chlorinated aliphatic hydrocarbons and chlorinated aromatic hydrocarbons (CHCs) are toxic and carcinogenic contaminants commonly found in environmental samples, and efficient online detection of these contaminants is still challenging at the present stage. Here, we report an advanced Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR) sensor for in-situ and simultaneous detection of multiple CHCs, including monochlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, trichloroethylene, perchloroethylene, and chloroform. The polycrystalline silver halide sensor fiber had a unique integrated planar-cylindric geometry, and was coated with an ethylene/propylene copolymer membrane to act as a solid phase extractor, which greatly amplified the analytical signal and contributed to a higher detection sensitivity compared to the previously reported sensors. This system exhibited a high detection sensitivity towards the CHCs mixture at a wide concentration range of 5~700 ppb. The FTIR-ATR sensor described in this study has a high potential to be utilized as a trace-sensitive on-line device for water contamination monitoring.

  19. Simultaneous wide-range stopping power determination for several ions

    Energy Technology Data Exchange (ETDEWEB)

    Alanko, T. E-mail: tommi.alanko@phys.jyu.fi; Trzaska, W.H.; Lyapin, V.; Raeisaenen, J.; Tiourine, G.; Virtanen, A

    2002-05-01

    A new procedure to extract simultaneously continuous stopping power curves for several ions and several absorbers over a wide energy range and with statistical errors reduced to negligible level is presented. The method combines our novel time-of-flight based method with the capability of our K130 cyclotron and ECR ion-source to produce the so-called ion cocktails. The potential of the method is demonstrated with a 6.0 MeV/u cocktail consisting of {sup 16}O{sup 4+}, {sup 28}Si{sup 7+} and {sup 40}Ar{sup 10+} ions. The stopping power in polycarbonate in the energy range of 0.35-5 MeV/u has been determined with absolute uncertainty of less than 2.3% and with relative below 0.2%. The results are compared with literature data and with SRIM2000 parameterisation including cores and bonds corrections.

  20. Simultaneous Determination of Caffeine and Vitamin B6 in Energy Drinks by High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Leacock, Rachel E.; Stankus, John J.; Davis, Julian M.

    2011-01-01

    A high-performance liquid chromatography experiment to determine the concentration of caffeine and vitamin B6 in sports energy drinks has been developed. This laboratory activity, which is appropriate for an upper-level instrumental analysis course, illustrates the standard addition method and simultaneous determination of two species. (Contains 1…

  1. Chemometrics-Assisted UV Spectrophotometric and RP-HPLC Methods for the Simultaneous Determination of Tolperisone Hydrochloride and Diclofenac Sodium in their Combined Pharmaceutical Formulation.

    Science.gov (United States)

    Gohel, Nikunj Rameshbhai; Patel, Bhavin Kiritbhai; Parmar, Vijaykumar Kunvarji

    2013-01-01

    Chemometrics-assisted UV spectrophotometric and RP-HPLC methods are presented for the simultaneous determination of tolperisone hydrochloride (TOL) and diclofenac sodium (DIC) from their combined pharmaceutical dosage form. Chemometric methods are based on principal component regression and partial least-square regression models. Two sets of standard mixtures, calibration sets, and validation sets were prepared. Both models were optimized to quantify each drug in the mixture using the information included in the UV absorption spectra of the appropriate solution in the range 241-290 nm with the intervals λ = 1 nm at 50 wavelengths. The optimized models were successfully applied to the simultaneous determination of these drugs in synthetic mixture and pharmaceutical formulation. In addition, an HPLC method was developed using a reversed-phase C18 column at ambient temperature with a mobile phase consisting of methanol:acetonitrile:water (60:30:10 v/v/v), pH-adjusted to 3.0, with UV detection at 275 nm. The methods were validated in terms of linearity, accuracy, precision, sensitivity, specificity, and robustness in the range of 3-30 μg/mL for TOL and 1-10 μg/mL for DIC. The robustness of the HPLC method was tested using an experimental design approach. The developed HPLC method, and the PCR and PLS models were used to determine the amount of TOL and DIC in tablets. The data obtained from the PCR and PLS models were not significantly different from those obtained from the HPLC method at 95% confidence limit.

  2. Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Dpto. Quimica Analitica, Nutricion y Bromatologia, Universidad de Santiago de Compostela (Spain)

    2001-08-01

    A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC-MIP-AES as measurement technique, were approximately 5-10 ng g{sup -1}. Precision in the consecutive analysis of three sediment samples varied between 3 and 10%. (orig.)

  3. Determination of the depth-resolved Stokes parameters of light backscattered from turbid media by use of polarization-sensitive optical coherence tomography

    International Nuclear Information System (INIS)

    Boer, J.F. de; Milner, T.E.; Nelson, J.S.

    1999-01-01

    Polarization-sensitive optical coherence tomography (PS-OCT) was used to characterize completely the polarization state of light backscattered from turbid media. Using a low-coherence light source, one can determine the Stokes parameters of backscattered light as a function of optical path in turbid media. To demonstrate the application of this technique we determined the birefringence and the optical axis in fibrous tissue (rodent muscle) and in vivo rodent skin. PS-OCT has potentially useful applications in biomedical optics by imaging simultaneously the structural properties of turbid biological materials and their effects on the polarization state of backscattered light. This method may also find applications in material science for investigation of polarization properties (e.g., birefringence) in opaque media such as ceramics and crystals. copyright 1999 Optical Society of America

  4. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

    2014-01-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg −1 for Mn to 77.3 mg kg −1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

  5. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

  6. Fast simultaneous determination of trimethoprim and sulfamethoxazole by capillary zone electrophoresis with capacitively coupled contactless conductivity detection.

    Science.gov (United States)

    da Silva, Iranaldo Santos; Vidal, Denis Tadeu Rajh; do Lago, Claudimir Lucio; Angnes, Lúcio

    2013-04-01

    The association of trimethoprim and sulfamethoxazole is a very effective with antibiotic properties, and commonly used in the treatment of a variety of infections. Due to the importance in diseases treatment of humans and also of animals, the development of methods for their quantification in commercial formulations is highly desirable. In the present study, a rapid method for simultaneous determination of these compounds using CE with capacitively coupled contactless conductivity detection was developed. A favorable working region for both analytes was from 12.5 to 200 μmol/L (linear responses with R > 0.999 for N = 5). Other parameters calculated were sensitivity (1.28 ± 0.10/1.45 ± 0.11) min/(μmol L), RSD (4.5%/2.0%), and LOD (1.1/3.3) μmol/L for trimethoprim and sulfamethoxazole, respectively. Under this condition, the total run time was only 2.6 min. The proposed method was applied to the determination of trimethoprim and sulfamethoxazole in commercial samples and the results were compared to those obtained by using a HPLC pharmacopoeia method. This new method is advantageous for quality-control analyses of trimethoprim and sulfamethoxazole in pharmaceuticals samples, because it is rapid and precise. Moreover, it is less laborious and demands minimum amounts of reagents in comparison to the recommended method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Simultaneous determination of the repertoire of classical neurotransmitters released from embryonal carcinoma stem cells using online microdialysis coupled with hydrophilic interaction chromatography–tandem mass spectrometry

    International Nuclear Information System (INIS)

    Tang, Ya-Bin; Sun, Fan; Teng, Lin; Li, Wen-Bin; An, Shi-Min; Zhang, Chun; Yang, Xin-Jie; Lv, Hao-Yu; Ding, Xu-Ping; Zhu, Liang

    2014-01-01

    Highlights: • An online MD-HILIC–MS/MS method for simultaneously measuring the repertoire of classical transmitters was developed and validated. • Hydrophilic interaction chromatography (HILIC) was successfully employed to online system. • Stable isotope labeled internal standards and authentic matrix have been applied to guarantee reliable results. • The method features simple procedure (no sample preparation), high recovery (≥73%), high accuracy (89.36% ≤ RE ≤ 116.89%), good reproducibility (2.18% ≤ RSD ≤ 14.56%), and sensitive limits of detection (2 pg for acetylcholine, serotonin, and glutamate, 10 pg for dopamine, norepinephrine, GABA, and glycine). - Abstract: Dynamic, continuous, and simultaneous multi-analysis of transmitters is important for the delineation of the complex interactions between the neuronal and intercellular communications. But the analysis of the whole repertoire of classical transmitters of diverse structure is challenging due to their different physico-chemical properties and to their high polarity feature which leads to poor retention in traditional reversed-phase columns during LC–MS analysis. Here, an online microdialysis coupled with hydrophilic interaction chromatography–tandem mass spectrometry (online MD-HILIC–MS/MS) detection method was developed for the simultaneous measurement of the repertoire of classical transmitters (acetylcholine, serotonin, dopamine, norepinephrine, glutamate, GABA, and glycine). Stable isotope labeled internal standards and authentic matrix have been applied to guarantee reliable results. The method was successfully employed to reveal the characteristics of transmitter release from embryonal carcinoma stem cells. The method features simple procedure (no sample preparation), high recovery (≥73%), high accuracy (89.36% ≤ RE ≤ 116.89%), good reproducibility (2.18% ≤ RSD ≤ 14.56%), and sensitive limits of detection (2 pg for acetylcholine, serotonin, and glutamate, 10 pg

  8. Simultaneous determination of the repertoire of classical neurotransmitters released from embryonal carcinoma stem cells using online microdialysis coupled with hydrophilic interaction chromatography–tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Ya-Bin [Department of Pharmacology and Chemical Biology, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Collaborative Innovation Center for Translational Medicine, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Sun, Fan [Department of Pharmacology and Chemical Biology, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Teng, Lin [Department of Pharmacology and Chemical Biology, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Department of Cardiology and Institute of Cardiovascular Diseases, The First College of Clinical Medical Sciences, China Three Gorges University, Yichang 443000, Hubei (China); Li, Wen-Bin; An, Shi-Min [Department of Pharmacology and Chemical Biology, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Collaborative Innovation Center for Translational Medicine, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Zhang, Chun; Yang, Xin-Jie; Lv, Hao-Yu; Ding, Xu-Ping [Department of Pharmacology and Chemical Biology, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Zhu, Liang, E-mail: zhuliang17@gmail.com [Department of Pharmacology and Chemical Biology, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); Collaborative Innovation Center for Translational Medicine, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025 (China); and others

    2014-11-07

    Highlights: • An online MD-HILIC–MS/MS method for simultaneously measuring the repertoire of classical transmitters was developed and validated. • Hydrophilic interaction chromatography (HILIC) was successfully employed to online system. • Stable isotope labeled internal standards and authentic matrix have been applied to guarantee reliable results. • The method features simple procedure (no sample preparation), high recovery (≥73%), high accuracy (89.36% ≤ RE ≤ 116.89%), good reproducibility (2.18% ≤ RSD ≤ 14.56%), and sensitive limits of detection (2 pg for acetylcholine, serotonin, and glutamate, 10 pg for dopamine, norepinephrine, GABA, and glycine). - Abstract: Dynamic, continuous, and simultaneous multi-analysis of transmitters is important for the delineation of the complex interactions between the neuronal and intercellular communications. But the analysis of the whole repertoire of classical transmitters of diverse structure is challenging due to their different physico-chemical properties and to their high polarity feature which leads to poor retention in traditional reversed-phase columns during LC–MS analysis. Here, an online microdialysis coupled with hydrophilic interaction chromatography–tandem mass spectrometry (online MD-HILIC–MS/MS) detection method was developed for the simultaneous measurement of the repertoire of classical transmitters (acetylcholine, serotonin, dopamine, norepinephrine, glutamate, GABA, and glycine). Stable isotope labeled internal standards and authentic matrix have been applied to guarantee reliable results. The method was successfully employed to reveal the characteristics of transmitter release from embryonal carcinoma stem cells. The method features simple procedure (no sample preparation), high recovery (≥73%), high accuracy (89.36% ≤ RE ≤ 116.89%), good reproducibility (2.18% ≤ RSD ≤ 14.56%), and sensitive limits of detection (2 pg for acetylcholine, serotonin, and glutamate, 10 pg

  9. Preparation of NiFe₂O₄/graphene nanocomposite and its application as a modifier for the fabrication of an electrochemical sensor for the simultaneous determination of tramadol and acetaminophen

    Energy Technology Data Exchange (ETDEWEB)

    Afkhami, Abbas, E-mail: afkhami@basu.ac.ir [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Khoshsafar, Hosein [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Bagheri, Hasan [Chemical Injuries Research Center, Baqiyatallah University of Medical Sciences, Tehran (Iran, Islamic Republic of); Madrakian, Tayyebeh [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of)

    2014-06-01

    Highlights: • A new modified electrochemical sensor was constructed and used. • NiFe₂O₄/graphene was used as the modifier. • The sensor was used for the determination of tramadol and acetaminophen in real samples. • Modification improved the sensitivity and detection limit of the method. • The oxidation of tramadol and acetaminophen at the surface of the electrode was studied. Abstract: An effective electrochemical sensor for the rapid and simultaneous determination of tramadol and acetaminophen based on carbon paste electrode (CPE) modified with NiFe₂O₄/graphene nanoparticles was developed. The structures of the synthesized NiFe₂O₄/graphene nanocomposite and the electrode composition were confirmed by X-ray diffraction (XRD) spectrometry, Fourier transform infrared (FT-IR) spectrometry and scanning electron microscopy (SEM). The peak currents of square wave voltammetry of tramadol and acetaminophen increased linearly with their concentration in the range of 0.01–9 μmol L⁻¹. The detection limit for their determination was found to be 0.0036 and 0.0030 μmol L⁻¹, respectively. The results show that the combination of graphene and NiFe₂O₄ nanoparticles causes a dramatic enhancement in the sensitivity of the sensor. The fabricated sensor exhibited high sensitivity and good stability, and would be valuable for the clinical assay of tramadol and acetaminophen.

  10. Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography-tandem mass spectrometry. The target compounds were preconcentrated by solid phase extraction. Pretreatment variables ...

  11. Simultaneous determination of ethanol's four types of non-oxidative metabolites in human whole blood by liquid chromatography tandem mass spectrometry

    DEFF Research Database (Denmark)

    Zhang, Xinyu; Zheng, Feng; Lin, Zebin

    2017-01-01

    The importance of ethanol non-oxidative metabolites as the specific biomarkers of alcohol consumption in clinical and forensic settings is increasingly acknowledged. Simultaneous determination of these metabolites can provide a wealth of information like drinking habit and history, but it was dif......The importance of ethanol non-oxidative metabolites as the specific biomarkers of alcohol consumption in clinical and forensic settings is increasingly acknowledged. Simultaneous determination of these metabolites can provide a wealth of information like drinking habit and history...

  12. Simultaneous determination of benznidazole and itraconazole using spectrophotometry applied to the analysis of mixture: A tool for quality control in the development of formulations

    Science.gov (United States)

    Pinho, Ludmila A. G.; Sá-Barreto, Lívia C. L.; Infante, Carlos M. C.; Cunha-Filho, Marcílio S. S.

    2016-04-01

    The aim of this work was the development of an analytical procedure using spectrophotometry for simultaneous determination of benznidazole (BNZ) and itraconazole (ITZ) in a medicine used for the treatment of Chagas disease. In order to achieve this goal, the analysis of mixtures was performed applying the Lambert-Beer law through the absorbances of BNZ and ITZ in the wavelengths 259 and 321 nm, respectively. Diverse tests were carried out for development and validation of the method, which proved to be selective, robust, linear, and precise. The lower limits of detection and quantification demonstrate its sensitivity to quantify small amounts of analytes, enabling its application for various analytical purposes, such as dissolution test and routine assays. In short, the quantification of BNZ and ITZ by analysis of mixtures had shown to be efficient and cost-effective alternative for determination of these drugs in a pharmaceutical dosage form.

  13. Simultaneous spectrophotometric determination of uranium and zirconium using cloud point extraction and multivariate methods

    International Nuclear Information System (INIS)

    Ghasemi, Jahan B.; Hashemi, Beshare; Shamsipur, Mojtaba

    2012-01-01

    A cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to simultaneous extraction and spectrophotometric determination of uranium and zirconium from aqueous solution using partial least squares (PLS) regression is investigated. The method is based on the complexation reaction of these cations with Alizarin Red S (ARS) and subsequent micelle-mediated extraction of products. The chemical parameters affecting the separation phase and detection process were studied and optimized. Under the optimum experimental conditions (i.e. pH 5.2, Triton X-114 = 0.20%, equilibrium time 10 min and cloud point 45 C), calibration graphs were linear in the range of 0.01-3 mg L -1 with detection limits of 2.0 and 0.80 μg L -1 for U and Zr, respectively. The experimental calibration set was composed of 16 sample solutions using an orthogonal design for two component mixtures. The root mean square error of predictions (RMSEPs) for U and Zr were 0.0907 and 0.1117, respectively. The interference effect of some anions and cations was also tested. The method was applied to the simultaneous determination of U and Zr in water samples.

  14. Monolayer covalent modification of 5-hydroxytryptophan on glassy carbon electrodes for simultaneous determination of uric acid and ascorbic acid

    International Nuclear Information System (INIS)

    Lin Xiangqin; Li Yongxin

    2006-01-01

    5-Hydroxytryptophan (5-HTP) was covalently grafted on the surface of glassy carbon electrodes (GCEs) using cyclic voltammetric method in a phosphate buffer solution. The prepared electrode, denoded as 5-HTP/GCE, was characterized by X-ray photoelectron spectroscopy, cyclic voltammetry and differential pulse voltammetry (DPV). Tryptophan grafted GCE (TRP/GCE) and 5-hydroxytryptamine grafted GCE (5-HTP/GCE) were also prepared by the same method for comparison. It was found that the electrocatalytic activities toward the oxidation of uric acid (UA) and ascorbic acid (AA) was in the order of 5-HT/GCE > 5-HTP/GCE > TRP/GCE for UA oxidation and 5-HT/GCE 5-HTP/GCE > TRP/GCE for AA oxidation. However, the CV current sensitivity was estimated as 4:2:1 for 5-HTP/GCE:5-HT/GCE:TRP/GCE. The DPV peaks for UA and AA oxidation appeared at 0.07 V and 0.34 V versus SCE, respectively, allowing simultaneous determination in mixtures. A linearly response in the range of: 5.0 x 10 -7 to 1.1 x 10 -5 M with the detection limit (s/n = 3) of 2.8 x 10 -7 M for UA determination, and a linear response in the range of: 5.0 x 10 -6 to 1.0 x 10 -4 M with the detection limit of 4.2 x 10 -6 M for AA determination were obtained. This electrode was used for UA and AA determinations in human urine samples satisfactorily

  15. Simultaneous determination of inorganic anions and cations in explosive residues by ion chromatography.

    Science.gov (United States)

    Meng, Hong-Bo; Wang, Tian-Ran; Guo, Bao-Yuan; Hashi, Yuki; Guo, Can-Xiong; Lin, Jin-Ming

    2008-07-15

    A non-suppressed ion chromatographic method by connecting anion-exchange and cation-exchange columns directly was developed for the separation and determination of five inorganic anions (sulfate, nitrate, chloride, nitrite, and chlorate) and three cations (sodium, ammonium, and potassium) simultaneously in explosive residues. The mobile phase was composed of 3.5mM phthalic acid with 2% acetonitrile and water at flow rate of 0.2 mL/min. Under the optimal conditions, the eight inorganic ions were completely separated and detected simultaneously within 16 min. The limits of detection (S/N=3) of the anions and cations were in the range of 50-100 microg/L and 150-320 microg/L, respectively, the linear correlation coefficients were 0.9941-0.9996, and the R.S.D. of retention time and peak area were 0.10-0.29% and 5.65-8.12%, respectively. The method was applied successfully to the analysis of the explosive samples with satisfactory results.

  16. Simultaneous RP-HPLC determination of sparfloxacin and dexamethasone in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    Syed Naeem Razzaq

    2013-06-01

    Full Text Available The present study describes the development and subsequent validation of simple and accurate stability indicating RP-HPLC method for the determination of sparfloxacin and dexamethasone in pharmaceutical formulations in the presence of their stress-induced degradation products. Both the drugs and their stress-induced degradation products were separated within 10 minutes using C8 column and mixture of methanol and 0.02 M phosphate buffer pH 3.0 (60:40 v/v, respectively as mobile phase at 270 nm using diode array detector. Regression analysis showed linearity in the range of 15-105 µg/mL for sparfloxacin and 5-35 µg/mL for dexamethasone. All the analytes were adequately resolved with acceptable tailing. Peak purity of the two drugs was also greater than 0.9999, showing no co-elution peaks. The developed method was applied for simultaneous determination of sparfloxacin and dexamethasone in pharmaceutical formulations for stability studies.

  17. Simultaneous determination of ethamsylate, tramadol and lidocaine in human urine by capillary electrophoresis with electrochemiluminescence detection.

    Science.gov (United States)

    Li, Jianguo; Ju, Huangxian

    2006-09-01

    Ethamsylate, tramadol and lidocaine, partly excreted by the kidney, are generally used as hemostatic, analgesic and local anesthetic in surgery. We developed a simple and sensitive method for their simultaneous monitoring in human urine based on CE coupled with electrochemiluminescence detection by end-column mode. Under optimized conditions the proposed method yielded linear ranges from 5.0 x 10(-8) to 5.0 x 10(-5), 1.0 x 10(-7) to 1.0 x 10(-4) and 1.0 x 10(-7) to 1.0 x 10(-4) M with LODs of 8.0 x 10(-9) M (36 amol), 1.6 x 10(-8) M (72 amol) and 1.0 x 10(-8) M (45 amol) (S/N = 3) for ethamsylate, tramadol and lidocaine, respectively. The RSD for their simultaneous detection at 1.0 x 10(-6) M was 2.1, 2.8 and 3.2% (n = 7), respectively. For practical application an extraction step with ethyl acetate at pH 11 was performed to eliminate the influence of the sample ionic strength. The recoveries of ethamsylate, tramadol and lidocaine at different levels in human urine were between 87 and 95%. This method was used for simultaneous detection of ethamsylate, tramadol and lidocaine in clinic urine samples from two medicated patients. It was valuable in clinical and biochemical laboratories for monitoring these drugs for various purposes.

  18. Multivariate Approaches for Simultaneous Determination of Avanafil and Dapoxetine by UV Chemometrics and HPLC-QbD in Binary Mixtures and Pharmaceutical Product.

    Science.gov (United States)

    2016-04-07

    Multivariate UV-spectrophotometric methods and Quality by Design (QbD) HPLC are described for concurrent estimation of avanafil (AV) and dapoxetine (DP) in the binary mixture and in the dosage form. Chemometric methods have been developed, including classical least-squares, principal component regression, partial least-squares, and multiway partial least-squares. Analytical figures of merit, such as sensitivity, selectivity, analytical sensitivity, LOD, and LOQ were determined. QbD consists of three steps, starting with the screening approach to determine the critical process parameter and response variables. This is followed by understanding of factors and levels, and lastly the application of a Box-Behnken design containing four critical factors that affect the method. From an Ishikawa diagram and a risk assessment tool, four main factors were selected for optimization. Design optimization, statistical calculation, and final-condition optimization of all the reactions were Carried out. Twenty-five experiments were done, and a quadratic model was used for all response variables. Desirability plot, surface plot, design space, and three-dimensional plots were calculated. In the optimized condition, HPLC separation was achieved on Phenomenex Gemini C18 column (250 × 4.6 mm, 5 μm) using acetonitrile-buffer (ammonium acetate buffer at pH 3.7 with acetic acid) as a mobile phase at flow rate of 0.7 mL/min. Quantification was done at 239 nm, and temperature was set at 20°C. The developed methods were validated and successfully applied for simultaneous determination of AV and DP in the dosage form.

  19. Affective evaluation of simultaneous tone combinations in congenital amusia.

    Science.gov (United States)

    Marin, Manuela M; Thompson, William Forde; Gingras, Bruno; Stewart, Lauren

    2015-11-01

    Congenital amusia is a neurodevelopmental disorder characterized by impaired pitch processing. Although pitch simultaneities are among the fundamental building blocks of Western tonal music, affective responses to simultaneities such as isolated dyads varying in consonance/dissonance or chords varying in major/minor quality have rarely been studied in amusic individuals. Thirteen amusics and thirteen matched controls enculturated to Western tonal music provided pleasantness ratings of sine-tone dyads and complex-tone dyads in piano timbre as well as perceived happiness/sadness ratings of sine-tone triads and complex-tone triads in piano timbre. Acoustical analyses of roughness and harmonicity were conducted to determine whether similar acoustic information contributed to these evaluations in amusics and controls. Amusic individuals' pleasantness ratings indicated sensitivity to consonance and dissonance for complex-tone (piano timbre) dyads and, to a lesser degree, sine-tone dyads, whereas controls showed sensitivity when listening to both tone types. Furthermore, amusic individuals showed some sensitivity to the happiness-major association in the complex-tone condition, but not in the sine-tone condition. Controls rated major chords as happier than minor chords in both tone types. Linear regression analyses revealed that affective ratings of dyads and triads by amusic individuals were predicted by roughness but not harmonicity, whereas affective ratings by controls were predicted by both roughness and harmonicity. We discuss affective sensitivity in congenital amusia in view of theories of affective responses to isolated chords in Western listeners. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

  20. Simultaneous determination of size and refractive index of red blood cells by light scattering measurements

    International Nuclear Information System (INIS)

    Ghosh, N.; Buddhiwant, P.; Uppal, A.; Majumder, S.K.; Patel, H.S.; Gupta, P.K.

    2006-01-01

    We present a fast and accurate approach for simultaneous determination of both the mean diameter and refractive index of a collection of red blood cells (RBCs). The approach uses the peak frequency of the power spectrum and the corresponding phase angle obtained by performing Fourier transform on the measured angular distribution of scattered light to determine these parameters. Results on the measurement of two important clinical parameters, the mean cell volume and mean cell hemoglobin concentration of a collection of RBCs, are presented

  1. Realization of ppm-level CO detection with exceptionally high sensitivity using reduced graphene oxide-loaded SnO2 nanofibers with simultaneous Au functionalization.

    Science.gov (United States)

    Kim, Jae-Hun; Katoch, Akash; Kim, Hyoun Woo; Kim, Sang Sub

    2016-03-07

    We have realized the highly sensitive, selective ppm-level carbon monoxide (CO) detection based on graphene oxide (RGO) nanosheets-loaded SnO2 nanofibers with simultaneous Au functionalization. The interplay between RGO/Au and SnO2 in terms of transfer of charge carriers and modulation of potential barriers is responsible for the exceptionally high CO detectability.

  2. Spectrophotometric studies on the complexation equilibria of Ni and Pb with 2-carboxy-2-hydroxy-5'-sulfo-formazylbenzene. Simultaneous determination of trace amounts of Ni and Pb.

    Science.gov (United States)

    Hashem, Elham Y; Abu-Bakr, Mohamed S; Hussain, Sawsan M

    2004-01-01

    Spectrophotometric studies have been made to investigate the reaction of Nickel and Lead with 2-carboxy-2'-hydroxy-5'-sulfoformazyl-benzene (zincon) in 50%(v/v) ethanol-water at 25 degrees C and an ionic strength of 0.1 M NaClO4. A complete picture of the complexation equilibria in the pH range (4.2-12.0) for nickel and (1.9-11.5) for lead are presented. Simple, rapid, selective and sensitive methods for the spectro-photometric determination of nickel and lead has been developed based on the color reaction of their complexes with zincon. The methods allow the determination of 4.69 microg mL(-1) of nickel at pH = 6.3 (lambdamax = 665 nm) and 10.3 microg ml(-1) of lead at pH = 5.6 (lambdamax = 610 nm). The apparent molar absorptivities were epsilon = 1.3 x 10(4) L mol(-1) cm(-1) for nickel and epsilon = 0.6 x 10(4) L mol(-1) cm(-1) for lead. The interference of a large number of foreign ions and complexing agents has been studied. Thiosulphate, as masking agent allows the simultaneous determination of nickel and lead in the presence of high concentrations of copper. Ascorbic acid, sodium cyanide and or sodium fluoride provide the elimination of many other interferences. The methods have been applied successfully to the simultaneous determination of nickel and lead in an aluminium and non-ferrous alloy.

  3. Application of Fourier transform near-infrared spectroscopy combined with high-performance liquid chromatography in rapid and simultaneous determination of essential components in crude Radix Scrophulariae.

    Science.gov (United States)

    Li, Xiaomeng; Fang, Dansi; Cong, Xiaodong; Cao, Gang; Cai, Hao; Cai, Baochang

    2012-12-01

    A method is described using rapid and sensitive Fourier transform near-infrared spectroscopy combined with high-performance liquid chromatography-diode array detection for the simultaneous identification and determination of four bioactive compounds in crude Radix Scrophulariae samples. Partial least squares regression is selected as the analysis type and multiplicative scatter correction, second derivative, and Savitzky-Golay filter were adopted for the spectral pretreatment. The correlation coefficients (R) of the calibration models were above 0.96 and the root mean square error of predictions were under 0.028. The developed models were applied to unknown samples with satisfactory results. The established method was validated and can be applied to the intrinsic quality control of crude Radix Scrophulariae.

  4. A novel electro analytical nanosensor based on graphene oxide/silver nanoparticles for simultaneous determination of quercetin and morin

    International Nuclear Information System (INIS)

    Yola, Mehmet Lütfi; Gupta, Vinod Kumar; Eren, Tanju; Şen, Arif Emre; Atar, Necip

    2014-01-01

    Graphical abstract: - Abstract: In this report, silver nanoparticles (AgNPs) with the mean diameters of 10-30 nm were self-assembled onto the surfaces of 2-aminoethanethiol (2-AET) functionalized graphene oxide (AETGO) sheets. The graphene oxide (GO) and AgNPs-AETGO nanocomposites were characterized by a transmission electron microscope (TEM), x-ray photoelectron spectroscopy (XPS), reflection–absorption infrared spectroscopy (RAIRS) and the x-ray diffraction (XRD). The simultaneous determination of quercetin (QR) and morin (MR) has been performed on glassy carbon electrode (GCE) modified with AgNPs-AETGO (AgNPs-AETGO/GCE). QR presented an oxidation step at Ea of 200 mV and reduction step at Ec of 150 mV and RT presented an oxidation step at Ea of 600 mV at AgNPs-AETGO/GCE by cyclic voltammetry (CV). The linearity ranges and the detection limits of QR and MR were 1.0 × 10-8 - 5.0 × 10-6 M and 3.3 × 10-9 M, respectively. The AgNPs-AETGO/GCE was also applied to real samples for the simultaneous determination of QR and MR. Thus the developed method can be adopted as an alternative to the published chromatographic, spectrophotometric and electroanalytical methods for simultaneous determination of QR and MR

  5. Electrochemical sensors for the simultaneous determination of zinc, cadmium and lead using a Nafion/ionic liquid/graphene composite modified screen-printed carbon electrode

    International Nuclear Information System (INIS)

    Chaiyo, Sudkate; Mehmeti, Eda; Žagar, Kristina; Siangproh, Weena; Chailapakul, Orawon; Kalcher, Kurt

    2016-01-01

    A simple, low cost, and highly sensitive electrochemical sensor, based on a Nafion/ionic liquid/graphene composite modified screen-printed carbon electrode (N/IL/G/SPCE) was developed to determine zinc (Zn(II)), cadmium (Cd(II)), and lead (Pb(II)) simultaneously. This disposable electrode shows excellent conductivity and fast electron transfer kinetics. By in situ plating with a bismuth film (BiF), the developed electrode exhibited well-defined and separate peaks for Zn(II), Cd(II), and Pb(II) by square wave anodic stripping voltammetry (SWASV). Analytical characteristics of the BiF/N/IL/G/SPCE were explored with calibration curves which were found to be linear for Zn(II), Cd(II), and Pb(II) concentrations over the range from 0.1 to 100.0 ng L"−"1. With an accumulation period of 120 s detection limits of 0.09 ng mL"−"1, 0.06 ng L"−"1 and 0.08 ng L"−"1 were obtained for Zn(II), Cd(II) and Pb(II), respectively using the BiF/N/IL/G/SPCE sensor, calculated as 3σ value of the blank. In addition, the developed electrode displayed a good repeatability and reproducibility. The interference from other common ions associated with Zn(II), Cd(II) and Pb(II) detection could be effectively avoided. Finally, the proposed analytical procedure was applied to detect the trace metal ions in drinking water samples with satisfactory results which demonstrates the suitability of the BiF/N/IL/G/SPCE to detect heavy metals in water samples and the results agreed well with those obtained by inductively coupled plasma mass spectrometry. - Highlights: • Nafion/ionic liquid/graphene composite modified electrode was fabricated. • Simultaneous determination of Zn, Cd and Pb in real samples was studied. • Zn, Cd and Pb could be sensitively measured as low as 90, 60 and 80 pg mL"−"1.

  6. Validation of a method for simultaneous determination of nitroimidazoles, benzimidazoles and chloramphenicols in swine tissues by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Xia, Xi; Wang, Yuanyuan; Wang, Xia; Li, Yun; Zhong, Feng; Li, Xiaowei; Huang, Yaoling; Ding, Shuangyang; Shen, Jianzhong

    2013-05-31

    This paper presents a sensitive and confirmatory multi-residue method for the analysis of 23 veterinary drugs and metabolites belonging to three classes (nitroimidazoles, benzimidazoles, and chloramphenicols) in porcine muscle, liver, and kidney. After extracted with ethyl acetate and basic ethyl acetate sequentially, the crude extracts were defatted with hexane and further purified using Oasis MCX solid-phase extraction cartridges. Rapid determination was carried out by ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Data acquisition was performed under positive and negative mode simultaneously. Recoveries based on matrix-matched calibrations for meat, liver, and kidney ranged from 50.6 to 108.1%. The method quantification limits were in the range of 3-100ng/kg. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. An Ion-pair Dispersive Liquid-Liquid Microextraction for Simultaneous Determination of Synthetic Dyes in Ice Cream Samples by HPLC

    Directory of Open Access Journals (Sweden)

    Mohammad Faraji

    2017-05-01

    Full Text Available An efficient, sensitive and fast method was developed based on an ultrasound-assisted extraction followed by an ion-pair dispersive liquid-liquid microextraction (USAE-IP-DLLME for the simultaneous determination of five commonly used synthetic sulfonate dyes (tartarazine, quinoline yellow, sunset yellow, azorubine, and brilliant blue in ice cream samples using high performance liquid chromatography. First, important parameters on USAE and samples clean-up were investigated and optimized. Then, some effective parameters on DLLME were studied and optimized. Under the optimum conditions, good linearity (0.5–1000 µg L-1, > r2=0.99 were obtained for the dyes. Limits of detection and limits of quantization were in the range of 0.01–0.05 µg L-1 and 0.03–0.15 µg L-1, respectively. The recoveries of the five synthetic colorants ranged from 90.3 to 109.7%. Intra (1.4–6.4% and inter-day precision (3.9–9.7% expressed as relative standard deviation (RSD at 10 and 100 µg L-1 levels less than 10% were also achieved. Finally, this method has been applied successfully in the determination of the colorants in the ice cream samples.

  8. Highly-sensitive electrocatalytic determination for toxic phenols based on coupled cMWCNT/cyclodextrin edge-functionalized graphene composite

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Juanjuan; Liu, Maoxiang [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Song, Haiou, E-mail: songhaiou2011@126.com [State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023 (China); Zhang, Shupeng, E-mail: shupeng_2006@126.com [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023 (China); Qian, Yueyue [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Li, Aimin, E-mail: liaimin@nju.edu.cn [State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210023 (China)

    2016-11-15

    Highlights: • Phenol detection based on coupled cMWCNT/CD edge-functionalized graphene composite. • Increased conductivity can inspire enhancement of electrocatalytic performance. • The synergistic combination of the trace amounts of CDs and cMWCNT is a pivotal. • GN-CD-cMWCNT shows an excellent electrocatalytic and anti-interference ability. - Abstract: Highly-sensitive electrocatalytic determination of toxic phenol compounds is of significance in environmental monitoring due to their low degradation and high toxicity to the environment and humans. In this paper, a rapid and sensitive electrochemical sensor based on coupled carboxyl-multi-walled carbon nanotube (cMWCNT) and cyclodextrin (CD) edge-functionalized graphene composite was successfully employed towards trace detection of three typical phenols (4-aminophenol, 4-AP; 4-chlorophenol, 4-CP; 4-nitrophenol, 4-NP). The morphology studies from scanning electron microscope and transmission electron microscope analysis revealed that cMWCNTs as conductive bridges were successfully incorporated into CD edge-functionalized graphene layers. Further, The electrocatalytic detection performance of the 3D simultaneously reduced and self-assembled sensing architecture (GN-CD-cMWCNT) with trace amounts of CDs was evaluated. The electrochemical studies demonstrated that GN-CD-cMWCNT displays excellent electrocatalytic activity, high sensitivity and stability. Under optimal conditions, the current responses of 4-AP, 4-CP and 4-NP are linear to concentrations over two different ranges, with low detection limit of 0.019, 0.017 and 0.027 μM (S/N = 3), respectively. And, GN-CD-cMWCNT shows an excellent anti-interference ability against electroactive species and metal ions. In addition, validation of the applicability of the presented sensor was also performed for the determination of three phenols in tap water sample with satisfactory results.

  9. Highly-sensitive electrocatalytic determination for toxic phenols based on coupled cMWCNT/cyclodextrin edge-functionalized graphene composite

    International Nuclear Information System (INIS)

    Gao, Juanjuan; Liu, Maoxiang; Song, Haiou; Zhang, Shupeng; Qian, Yueyue; Li, Aimin

    2016-01-01

    Highlights: • Phenol detection based on coupled cMWCNT/CD edge-functionalized graphene composite. • Increased conductivity can inspire enhancement of electrocatalytic performance. • The synergistic combination of the trace amounts of CDs and cMWCNT is a pivotal. • GN-CD-cMWCNT shows an excellent electrocatalytic and anti-interference ability. - Abstract: Highly-sensitive electrocatalytic determination of toxic phenol compounds is of significance in environmental monitoring due to their low degradation and high toxicity to the environment and humans. In this paper, a rapid and sensitive electrochemical sensor based on coupled carboxyl-multi-walled carbon nanotube (cMWCNT) and cyclodextrin (CD) edge-functionalized graphene composite was successfully employed towards trace detection of three typical phenols (4-aminophenol, 4-AP; 4-chlorophenol, 4-CP; 4-nitrophenol, 4-NP). The morphology studies from scanning electron microscope and transmission electron microscope analysis revealed that cMWCNTs as conductive bridges were successfully incorporated into CD edge-functionalized graphene layers. Further, The electrocatalytic detection performance of the 3D simultaneously reduced and self-assembled sensing architecture (GN-CD-cMWCNT) with trace amounts of CDs was evaluated. The electrochemical studies demonstrated that GN-CD-cMWCNT displays excellent electrocatalytic activity, high sensitivity and stability. Under optimal conditions, the current responses of 4-AP, 4-CP and 4-NP are linear to concentrations over two different ranges, with low detection limit of 0.019, 0.017 and 0.027 μM (S/N = 3), respectively. And, GN-CD-cMWCNT shows an excellent anti-interference ability against electroactive species and metal ions. In addition, validation of the applicability of the presented sensor was also performed for the determination of three phenols in tap water sample with satisfactory results.

  10. Simultaneous Determination of 11 Compounds in Gualou Guizhi Granule and Pharmacokinetics Study by UPLC-MS/MS

    Directory of Open Access Journals (Sweden)

    Chengtao Sun

    2017-01-01

    Full Text Available A rapid and sensitive ultrafast performance liquid chromatography-tandem mass spectrometry method (UPLC-MS/MS was developed for the simultaneous determination of 11 compounds in Gualou Guizhi Granule (GLGZG, including liquiritin, isoliquiritin, liquirtin apioside, isoliquiritin apioside, liquiritigenin, isoliquiritigenin, glycyrrhizic acid, glycyrrhetinic acid, paeoniflorin, albiflorin, and paeoniflorin sulfonate in rat plasma. UPLC-MS/MS assay with negative ion mode was performed on a Waters CORTECS C18 (2.1 × 100 mm, 1.6 μm with the mobile phase consisting of 0.1% aqueous formic acid (A and acetonitrile (B in gradient elution at a flow rate of 0.25 mL·min−1. The method was linear for all analytes within the detection range (r≥0.9597. The inter- and intraday precision (RSD were 2.21–6.41% and 1.67–6.18%; the inter- and intraday accuracy (recover were 92.48–114.03% and 90.23–112.04%. And the recovery rate ranged from 81.30% to 108.22%. The matrix effect values obtained for analytes ranged from 88.91% to 113.32%. This validated method was successfully applied to a pharmacokinetics study in rats after oral administration of GLGZG.

  11. A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

    Directory of Open Access Journals (Sweden)

    Ali S. Abdelhameed

    2014-01-01

    Full Text Available A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear with r2=0.9999 for PTZ and r2=0.9995 for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1 for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1 for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD <7.76% for PTZ and <7.58 % for ETD.

  12. Development and Validation of RP-HPLC Method for the Simultaneous Determination of Rabeprazole Sodium and Itopride Hydrochloride in Solid Dosage Form

    Directory of Open Access Journals (Sweden)

    Rajesh Sharma

    2010-01-01

    Full Text Available A simple, sensitive, precise, accurate, rapid and reproducible reverse phase high performance liquid chromatographic procedure is developed for simultaneous determination of rabeprazole sodium and itopride hydrochloride in solid dosage form. The mobile phase used was a combination of acetonitrile: buffer (35:65 v/v and the pH was adjusted to 7.0 ± 0.1 by addition of triethylamine. The detection of the capsule dosage form was carried out at 266 nm and a flow rate employed was 1 mL/min. Linearity was obtained in the concentration range of 2 to 16 μg/mL of rabeprazole sodium and 5 to 55 μg/mL of itopride hydrochloride with a correlation coefficient of 0.9992 and 0.9996 respectively. The results of the analysis were validated statistically and recovery studies confirmed the accuracy of the proposed method.

  13. Study on performance of a simultaneous spectrometer of ICP emission source for the determination of the major elements in rocks

    International Nuclear Information System (INIS)

    Vieira, M.D.

    1987-01-01

    The optimization of operational parameters of a simultaneous spectrometer coupled to an ICP excitation source in order to establish an analytical method for the simultaneous determination of the major elements in rocks is studied. The mutual spectral interferences, calibration curves for the acid and saline matrix and the internal standard method with ytrium are analyzed. (M.J.C.) [pt

  14. Simultaneous Determination of Four Preservatives in Foodstuffs by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Mohammad Faraji

    2016-04-01

    Full Text Available Background and objectives:  High concentration of preservatives in food may result in gastrointestinal disturbances whereby some patients suffering from asthma, rhinitis, or urticaria. The aim of this study is the introduction and optimization a new method for simultaneous determination of four preservatives (SB, PS, MP, PP in foodstuff by high performance liquid chromatography. Materials and methods: Important factors in extraction, separation and determination process were optimized using the one variable at a time method.  Figures of merit of the proposed method were evaluated. The amount of SB, PS, MP, PP in some food samples were determined using the proposed method. Result: The results showed that the obtained chromatogram of extract was free of significant interferences. The preservatives recoveries ranged from 88% to 110 %. Concentration of SB, PS, MP and PP in the 20studied samples ranges between N.D-639.9, N.D -214.5, N.D -579.8 and N.D -30.5 mg kg-1, respectively  Conclusion: The performance and reliability of proposed method as a simple, efficient and fast method for determination of SB, PS, MP, PP in the food samples was demonstrated.

  15. Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers

    International Nuclear Information System (INIS)

    Srapeniants, R.A.; Saveliev, I.B.; Kovtun, J.L.; Sidorov, A.V.; Tsagolov, K.S.; Miroshnikova, N.N.

    1982-01-01

    A radioactivation method for the simultaneous determination of the nitrogen, phosphorus and potassium content in plants and fertilizers is described. Samples to be analyzed and standard samples are exposed to neutron irradiation, and the spectra of gamma radiation induced in the samples are recorded. The samples laid aside for a period of time determined by the half-life of interfering isotopes, and the spectra of the samples and standards are recorded again. The first and second spectra are superposed and shifted relative to each other along the energy axis, and the content of the elements being analyzed is determined by comparing the spectra of the samples and standards

  16. Sensitivity determination of CR-39 from Normal and inclined incidence

    International Nuclear Information System (INIS)

    Abou, A.A.; El-Kheir, A.A.; Daas, A.F.; Awwad, Z.; Reda, A.M.

    2000-01-01

    An experimental study have been carried out on alpha- particle track opening (Major and minor axes) using alpha-particles of different energies incident with different angels in addition to the normal incidence. The sensitivity of CR-39 in present work is determined for each of normal and inclined incidence. The results indicated a difference in the sensitivity according to angle of incidence. The variation of alpha- particle tracks (major and minor axes) are calculated and compared with our measured values. Also, it is found that the sensitivity of CR-39 detector is change due to the storage time at room temperature

  17. A novel bi-enzyme electrochemical biosensor for selective and sensitive determination of methyl salicylate.

    Science.gov (United States)

    Fang, Yi; Umasankar, Yogeswaran; Ramasamy, Ramaraja P

    2016-07-15

    An amperometric sensor based on a bi-enzyme modified electrode was fabricated to detect methyl salicylate, a volatile organic compound released by pathogen-infected plants via systemic response. The detection is based on cascadic conversion reactions that result in an amperometric electrochemical signal. The bi-enzyme electrode is made of alcohol oxidase and horseradish peroxidase enzymes immobilized on to a carbon nanotube matrix through a molecular tethering method. Methyl salicylate undergoes hydrolysis to form methanol, which is consumed by alcohol oxidase to form formaldehyde while simultaneously reducing oxygen to hydrogen peroxide. The hydrogen peroxide will be further reduced to water by horseradish peroxidase, which results in an amperometric signal via direct electron transfer. The bi-enzyme biosensor was evaluated by cyclic voltammetry and constant potential amperometry using hydrolyzed methyl salicylate as the analyte. The sensitivity of the bi-enzyme biosensor as determined by cyclic voltammetry and constant potential amperometry were 112.37 and 282.82μAcm(-2)mM(-1) respectively, and the corresponding limits of detection were 22.95 and 0.98μM respectively. Constant potential amperometry was also used to evaluate durability, repeatability and interference from other compounds. Wintergreen oil was used for real sample study to establish the application of the bi-enzyme sensor for selective determination of plant pathogen infections. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Simultaneous Determination of Four Anthraquinones in Polygoni Multiflori Radix with Single Reference Standard by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hua Yang

    2015-07-01

    Full Text Available Objective: To establish a rapid, accurate and reliable analytical method for the simultaneous determination of four major anthraquinones in Polygoni Multiflori Radix (PMR using single reference standard.

  19. Simultaneous determination of benznidazole and itraconazole using spectrophotometry applied to the analysis of mixture: A tool for quality control in the development of formulations.

    Science.gov (United States)

    Pinho, Ludmila A G; Sá-Barreto, Lívia C L; Infante, Carlos M C; Cunha-Filho, Marcílio S S

    2016-04-15

    The aim of this work was the development of an analytical procedure using spectrophotometry for simultaneous determination of benznidazole (BNZ) and itraconazole (ITZ) in a medicine used for the treatment of Chagas disease. In order to achieve this goal, the analysis of mixtures was performed applying the Lambert-Beer law through the absorbances of BNZ and ITZ in the wavelengths 259 and 321 nm, respectively. Diverse tests were carried out for development and validation of the method, which proved to be selective, robust, linear, and precise. The lower limits of detection and quantification demonstrate its sensitivity to quantify small amounts of analytes, enabling its application for various analytical purposes, such as dissolution test and routine assays. In short, the quantification of BNZ and ITZ by analysis of mixtures had shown to be efficient and cost-effective alternative for determination of these drugs in a pharmaceutical dosage form. Copyright © 2016. Published by Elsevier B.V.

  20. A glassy carbon electrode modified with cerium phosphate nanotubes for the simultaneous determination of hydroquinone, catechol and resorcinol.

    Science.gov (United States)

    Li, Zhen; Yue, Yuhua; Hao, Yanjun; Feng, Shun; Zhou, Xianli

    2018-03-12

    A nafion film containing cerium phosphate nanotubes was pasted onto a glassy carbon electrode (GCE) to obtain a sensor for hydroquinone (HQ). The morphologies and components of the coating were characterized by transmission electron microscopy, scanning electron microscopy and energy-dispersive spectroscopy. Cyclic voltammetry and differential pulse voltammetry (DPV) showed the specific surface of the electrode to be significantly increased and the electron transfer rate to be accelerated. The modified GCE was applied to the determination of hydroquinone (HQ) via DPV. The oxidation current increases linearly in the 0.23 μM to 16 mM HQ concentration range which is as wide as five orders of magnitude. The limit of detection is 0.12 μM (based on a signal-to-noise ratio of 3), and the sensitivity is 1.41 μA·μM -1  cm -2 . The method was further applied to the simultaneous determination of HQ, catechol and resorcinol. The potentials for the three species are well separated (20, 134, and 572 mV vs SCE). Average recoveries from (spiked) real water samples are between 95.2 and 107.0%, with relative standard deviations of 0.9~2.7% (for n = 3) at three spiking levels. The method was validated by independent assays using HPLC. Graphical abstract ᅟ.

  1. Net Analyte Signal Standard Additions Method for Simultaneous Determination of Sulfamethoxazole and Trimethoprim in Pharmaceutical Formulations and Biological Fluids

    OpenAIRE

    Givianrad, M. H.; Mohagheghian, M.

    2012-01-01

    The applicability of a novel net analyte signal standard addition method (NASSAM) to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim was verified by UV-visible spectrophotometry. The results confirmed that the net analyte signal standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. Moreover, applying the net analyte signal standard a...

  2. Simultaneous Determination of 14 Phenolic Compounds in Grape Canes by HPLC-DAD-UV Using Wavelength Switching Detection

    Directory of Open Access Journals (Sweden)

    Ang Zhang

    2013-11-01

    Full Text Available The paper described a novel chromatographic method for the simultaneous determination of phenolic compounds such as gallic, protocatechuic, vanillic, caffeic, syringic, p-coumaric and salicylic acid, (+-catechin, (‒-epicatechin, rutin, morin, quercetin, coumarin and trans-resveratrol at their maximum absorbance wavelengths (MAW employing reverse-phase high performance liquid chromatography combined with DAD and UV detection via detection wavelength switching. The method was based on MAW acquisition by DAD and quantification by UV. The separation process was performed on a Shim-Pack VP-ODS C18 column (250 mm × 4.6 mm, 5 μm held at 30 °C, utilizing 3.0% acetic acid and acetonitrile as mobile phase at a flow rate of 0.8 mL/min in the gradient elution mode. The method was fully validated in terms of linearity (r2 > 0.9990, 10‒350 mg/L, precision (both intra-day and inter-day RSD < 4.22%, accuracy (97.31%‒104.66%, specificity, robustness (0.59% < RSD < 2.86%, limit of detection and quantification. The switching method significantly improved the sensitivities of most phenolics studied in comparison with the standard constant wavelength detection (280 nm. The proposed method has been successfully applied to the determination of 14 phenolic compounds in 89 varieties of one-year-old Chinese grape one-year-canes. Grape canes contain many phenolics, especially trans-resveratrol, (‒-epicatechin, and (+-catechin.

  3. MICROORGANISMS ANTIBIOTIC SENSITIVITY DETERMINATION IN URINARY TRACT INFECTIONS

    Directory of Open Access Journals (Sweden)

    Shapovalova O.V.

    2016-06-01

    Full Text Available Introduction. Nowadays Urinary tract infections (UTI are considered to be the most common bacterial infections. Escherichia coli is the most frequently uropathogen. Other microorganisms of the genera Enterococcus, Klebsiella, Enterobacter, Proteus, Morganella, Citrobacter, Serratia, Pseudomonas, Streptococcus, Staphylococcus, Candida are also isolated with variable frequency. In recent years there has been a decreasing tendency of the causative agents of UTI sensitivity to various antibiotics, which causes growth of an inefficiency treatment risk. In connection with the above the investigations were carried out with the purpose to identify the actual causative agents of bacteriuria and their sensitivity to antibiotics and antifungal drugs. Materials and methods. Bacteriological examination of urine was performed at 42 patients of SI "Sytenko Institute of Spine and Joint Pathology, AMS of Ukraine" clinic. The bacteriological method for determining the number of bacteria in the test material, cultural and bacterioscopic methods for identifying microorganisms and disk-diffusion method for sensitivity of microorganisms to antibiotics determining were used. The clinical material for the study was an average portion of the morning urine or urine collected by catheter. The biological material collection and bacteriological examination was carried by quantitative method, the isolated microorganisms identification and their sensitivity to antibiotics determining was performed by standard methods in accordance with current guidelines. We used the following antibiotics group to determine the microorganisms sensitivity: penicillin, cephalosporin, karbapenems, tetracyclines, aminoglycoside, fluoroquinolones, oxazolidinones, macrolides, lincosamides, glycopeptides, antifungal antibiotics. Results and discussion. During the biological material study 55 isolates of bacterial and fungal pathogens were obtained. The microorganisms’ concentration in urine was in

  4. A Sensitive Validated Spectrophotometric Method for the Determination of Flucloxacillin Sodium

    Directory of Open Access Journals (Sweden)

    R. Singh Gujral

    2009-01-01

    Full Text Available A simple and sensitive spectrophotometric method has been proposed for the determination of flucloxacillin sodium. The determination method is based on charge transfer complexation reaction of the drug with iodine in methanol-dichloromethane medium. The absorbance was measured at 362 nm against the reagent blank. Under optimized experimental conditions, Beer's law is obeyed in the concentration ranges 1-9 μg/mL for flucloxacillin. The method was validated for specificity, linearity, precision, accuracy. The degree of linearity of the calibration curves, the percent recoveries, limit of detection and quantitation for the spectrophotometric method were determined. No interferences could be observed from the additives commonly present in the pharmaceutical formulations. The method was successfully applied for in vitro determination of human urine samples with low RSD value. This is simple, specific, accurate and sensitive spectrophotometric method.

  5. Preparation of NiFe2O4/graphene nanocomposite and its application as a modifier for the fabrication of an electrochemical sensor for the simultaneous determination of tramadol and acetaminophen

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Khoshsafar, Hosein; Bagheri, Hasan; Madrakian, Tayyebeh

    2014-01-01

    Highlights: • A new modified electrochemical sensor was constructed and used. • NiFe 2 O 4 /graphene was used as the modifier. • The sensor was used for the determination of tramadol and acetaminophen in real samples. • Modification improved the sensitivity and detection limit of the method. • The oxidation of tramadol and acetaminophen at the surface of the electrode was studied. - Abstract: An effective electrochemical sensor for the rapid and simultaneous determination of tramadol and acetaminophen based on carbon paste electrode (CPE) modified with NiFe 2 O 4 /graphene nanoparticles was developed. The structures of the synthesized NiFe 2 O 4 /graphene nanocomposite and the electrode composition were confirmed by X-ray diffraction (XRD) spectrometry, Fourier transform infrared (FT-IR) spectrometry and scanning electron microscopy (SEM). The peak currents of square wave voltammetry of tramadol and acetaminophen increased linearly with their concentration in the range of 0.01–9 μmol L −1 . The detection limit for their determination was found to be 0.0036 and 0.0030 μmol L −1 , respectively. The results show that the combination of graphene and NiFe 2 O 4 nanoparticles causes a dramatic enhancement in the sensitivity of the sensor. The fabricated sensor exhibited high sensitivity and good stability, and would be valuable for the clinical assay of tramadol and acetaminophen

  6. Sensitive determination of trace mercury by UV-visible diffuse reflectance spectroscopy after complexation and membrane filtration-enrichment.

    Science.gov (United States)

    Yin, Changhai; Iqbal, Jibran; Hu, Huilian; Liu, Bingxiang; Zhang, Lei; Zhu, Bilin; Du, Yiping

    2012-09-30

    A simple, sensitive and selective solid phase reflectometry method is proposed for the determination of trace mercury in aqueous samples. The complexation reagent dithizone was firstly injected into the properly buffered solution with vigorous stirring, which started a simultaneous formation of nanoparticles suspension of dithizone and its complexation reaction with the mercury(II) ions to make Hg-dithizone nanoparticles. After a definite time, the mixture was filtered with membrane, and then quantified directly on the surface of the membrane by using integrating sphere accessory of the UV-visible spectrophotometer. The quantitative analysis was carried out at a wavelength of 485 nm since it yielded the largest difference in diffuse reflectance spectra before and after reaction with mercury(II).A good linear correlation in the range of 0.2-4.0 μg/L with a squared correlation coefficient (R(2)) of 0.9944 and a detection limit of 0.12 μg/L were obtained. The accuracy of the method was evaluated by the analysis of spiked mercury(II) concentrations determined using this method along with those determined by the atomic fluorescence mercury vapourmeter and the results obtained were in good agreement. The proposed method was applied to the determination of mercury in tap water and river water samples with the recovery in an acceptable range (95.7-105.3%). Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Fabrication and application of a new modified electrochemical sensor using nano-silica and a newly synthesized Schiff base for simultaneous determination of Cd2+, Cu2+ and Hg2+ ions in water and some foodstuff samples

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Soltani-Felehgari, Farzaneh; Madrakian, Tayyebeh; Ghaedi, Hamed; Rezaeivala, Majid

    2013-01-01

    Highlights: ► A new modified electrochemical sensor was constructed and used. ► A new Schiff base coated nano-silica was used as modifier. ► The electrochemical properties of electrode were studied. ► This modifier enhanced the electrochemical properties of electrode. ► The electrode was used for simultaneous determination of Cd 2+ , Cu 2+ and Hg 2+ ions. -- Abstract: A new chemically modified carbon paste electrode was constructed and used for rapid, simple, accurate, selective and highly sensitive simultaneous determination of cadmium, copper and mercury using square wave anodic stripping voltammetry (SWASV). The carbon paste electrode was modified by N,N′-bis(3-(2-thenylidenimino)propyl)piperazine coated silica nanoparticles. Compared with carbon paste electrode, the stripping peak currents had a significant increase at the modified electrode. Under the optimized conditions (deposition potential, −1.100 V vs. Ag/AgCl; deposition time, 60 s; resting time, 10 s; SW frequency, 25 Hz; pulse amplitude, 0.15 V; dc voltage step height, 4.4 mV), the detection limit was 0.3, 0.1 and 0.05 ng mL −1 for the determination of Cd 2+ , Cu 2+ and Hg 2+ , respectively. The complexation reaction of the ligand with several metal cations in methanol was studied and the stability constants of the complexes were obtained. The effects of different cations and anions on the simultaneous determination of metal ions were studied and it was found that the electrode is highly selective for the simultaneous determination of Cd 2+ , Cu 2+ and Hg 2+ . Furthermore, the present method was applied to the determination of Cd 2+ , Cu 2+ and Hg 2+ in water and some foodstuff samples

  8. Simultaneous determination of aquifer parameters and zone structures with fuzzy c-means clustering and meta-heuristic harmony search algorithm

    Science.gov (United States)

    Ayvaz, M. Tamer

    2007-11-01

    This study proposes an inverse solution algorithm through which both the aquifer parameters and the zone structure of these parameters can be determined based on a given set of observations on piezometric heads. In the zone structure identification problem fuzzy c-means ( FCM) clustering method is used. The association of the zone structure with the transmissivity distribution is accomplished through an optimization model. The meta-heuristic harmony search ( HS) algorithm, which is conceptualized using the musical process of searching for a perfect state of harmony, is used as an optimization technique. The optimum parameter zone structure is identified based on three criteria which are the residual error, parameter uncertainty, and structure discrimination. A numerical example given in the literature is solved to demonstrate the performance of the proposed algorithm. Also, a sensitivity analysis is performed to test the performance of the HS algorithm for different sets of solution parameters. Results indicate that the proposed solution algorithm is an effective way in the simultaneous identification of aquifer parameters and their corresponding zone structures.

  9. Electrochemical sensor based on graphene and mesoporous TiO2 for the simultaneous determination of trace colourants in food.

    Science.gov (United States)

    Gan, Tian; Sun, Junyong; Meng, Wen; Song, Li; Zhang, Yuxia

    2013-12-15

    Currently, synthetic colourants draw much attention as food additives. This paper investigated the simultaneous electrocatalytic oxidation of sunset yellow and tartrazine, two yellow colourants commonly present in food together, with a novel voltammetric sensor based on graphene and mesoporous TiO2 modified carbon paste electrode. Due to the high accumulation effect and great catalytic capability of graphene and mesoporous TiO2, the developed sensor exhibited well-defined and separate square wave voltammetric peaks (i.e., 272 mV) for sunset yellow tartrazine. The peak currents of sunset yellow and tartrazine increased linearly with their concentration in the ranges of 0.02-2.05 μM and 0.02-1.18 μM, respectively. And the detection limit was 6.0 and 8.0 nM for sunset yellow and tartrazine, respectively. This new sensor was applied to determine sunset yellow and tartrazine in several food sample extracts. Results suggested that the proposed sensor was sensitive, rapid and reliable. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. Simultaneous determination of 13 carbohydrates using high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry.

    Science.gov (United States)

    Zhao, Dan; Feng, Feng; Yuan, Fei; Su, Jin; Cheng, Yan; Wu, Hanqiu; Song, Kun; Nie, Bo; Yu, Lian; Zhang, Feng

    2017-04-01

    A simple, accurate, and highly sensitive method was developed for the determination of 13 carbohydrates in polysaccharide of Spirulina platensis based on high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry. Samples were extracted with deionized water using ultrasonic-assisted extraction, and the ultrasound-assisted extraction conditions were optimized by Box-Behnken design. Then the extracted polysaccharide was hydrolyzed by adding 1 mol/L trifluoroacetic acid before determination by high-performance anion-exchange chromatography coupled with pulsed amperometric detection and confirmed by high-performance anion-exchange chromatography coupled with mass spectrometry. The high-performance anion-exchange chromatography coupled with pulsed amperometric detection method was performed on a CarboPac PA20 column by gradient elution using deionized water, 0.1 mol/L sodium hydroxide solution, and 0.4 mol/L sodium acetate solution. Excellent linearity was observed in the range of 0.05-10 mg/L. The average recoveries ranged from 80.7 to 121.7%. The limits of detection and limits of quantification for 13 carbohydrates were 0.02-0.10 and 0.2-1.2  μg/kg, respectively. The developed method has been successfully applied to ambient samples, and the results indicated that high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry could provide a rapid and accurate method for the simultaneous determination of carbohydrates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Development of a novel running buffer for the simultaneous determination of nitrate and nitrite in human serum by capillary zone electrophoresis.

    Science.gov (United States)

    Miyado, Takashi; Nagai, Hidenori; Takeda, Sahori; Saito, Keiitsu; Fukushi, Keiichi; Yoshida, Yasukazu; Wakida, Shin-ichi; Niki, Etsuo

    2003-10-03

    In order to improve NO2- peak height and obtain a convenient buffer system for the assay of nitrogen monooxide metabolites, we developed a novel running buffer for the simultaneous determination of nitrite and nitrate in human serum by capillary electrophoresis. The addition of cetyltrimethylammonium chloride to the running buffer resulted in high-speed separation using reverse electroosmotic flow. Highly sensitive determination was also achieved using stacking with 10-fold diluted sample solutions. The samples were injected hydrodynamically for 100 s into a 50 cm x 75 microm I.D. capillary. The separation voltage was 10 kV (negative polarity). UV detection was performed at 214 nm. We obtained complete separation of nitrite and nitrate in deproteinized human serum within 6 min with optimum analytical conditions. Linear calibration curves for nitrite and nitrate for both peak height and peak area were obtained with standard addition method. The limits of detection obtained at a signal-to-noise ratio of 3 for nitrite and nitrate were 4.1 and 2.0 microM, while the values of relative standard deviation of peak height were 2.4 and 2.6%, respectively.

  12. Simultaneous determination of 56 Mn and 187W in neutron activated steels

    International Nuclear Information System (INIS)

    Melo, M.C. de

    1982-01-01

    The simultaneous determination of the count rates due to 56 Mn and 187 W in the activation analysis of steel samples was carried out through exponential regression using least square fitting. The regression coefficients obtained corresponded to the initial count rates of 56 Mn and 187 W. Later on, the count rates of 56 Mn were correlated to the manganese content in the samples and to the count rates of the same radionuclide, obtained in a region of the gamma spectrum where only 56 Mn was apparent. The correlation coefficients were respectively .968 and .99997, thus demonstrating the applicability of the methodology adopted herein. (Author) [pt

  13. Simultaneous determination of Albendazol and Triclabendazole in Triclazol 22 suspension for veterinary purposes

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad Margarita; Gafas Leyva, Maite; Rosales Bosch, Karina

    2013-01-01

    To validate the analytical method for simultaneous determination of triclabendazole and al bendazole in triclazol 22 suspension for quality control. For quantitation of the active principle in the final product, the separation was performed through a liquid chromatographic column Lichrosorb RP-18 (5 μm) (250 x 4 mm), with ultraviolet detection range of 298 nm, by using a mobile phase of acetonitrile: ammonium acetate buffer solution of ph 6.6 (70:30); the quantitation was made against a reference sample by means of the external standard method

  14. A method to simultaneously determining the reduction in PAH dissolved concentrations and bioaccessibility in carbon amended soils

    DEFF Research Database (Denmark)

    Marchal, Geoffrey; Smith, Kilian E. C.; Rein, Arno

    In order to investigate the potential of different soil amendments (activated charcoal (AC), charcoal (biochar), compost) to sorb PAHs and their effect on bioaccessibility and biodegradation of PAHs in soil, a method was developed that can determine simultaneously the changes in PAH dissolved...

  15. Simultaneous pH-sensitive and oxygen-sensitive MRI of human gliomas at 3 T using multi-echo amine proton chemical exchange saturation transfer spin-and-gradient echo echo-planar imaging (CEST-SAGE-EPI).

    Science.gov (United States)

    Harris, Robert J; Yao, Jingwen; Chakhoyan, Ararat; Raymond, Catalina; Leu, Kevin; Liau, Linda M; Nghiemphu, Phioanh L; Lai, Albert; Salamon, Noriko; Pope, Whitney B; Cloughesy, Timothy F; Ellingson, Benjamin M

    2018-04-06

    To introduce a new pH-sensitive and oxygen-sensitive MRI technique using amine proton CEST echo spin-and-gradient echo (SAGE) EPI (CEST-SAGE-EPI). pH-weighting was obtained using CEST estimations of magnetization transfer ratio asymmetry (MTR asym ) at 3 ppm, and oxygen-weighting was obtained using R2' measurements. Glutamine concentration, pH, and relaxation rates were varied in phantoms to validate simulations and estimate relaxation rates. The values of MTR asym and R2' in normal-appearing white matter, T 2 hyperintensity, contrast enhancement, and macroscopic necrosis were measured in 47 gliomas. Simulation and phantom results confirmed an increase in MTR asym with decreasing pH. The CEST-SAGE-EPI estimates of R 2 , R2*, and R2' varied linearly with gadolinium diethylenetriamine penta-acetic acid concentration (R 2  = 6.2 mM -1 ·sec -1 and R2* = 6.9 mM -1 ·sec -1 ). The CEST-SAGE-EPI and Carr-Purcell-Meiboom-Gill estimates of R 2 (R 2  = 0.9943) and multi-echo gradient-echo estimates of R2* (R 2  = 0.9727) were highly correlated. T 2 lesions had lower R2' and higher MTR asym compared with normal-appearing white matter, suggesting lower hypoxia and high acidity, whereas contrast-enhancement tumor regions had elevated R2' and MTR asym , indicating high hypoxia and acidity. The CEST-SAGE-EPI technique provides simultaneous pH-sensitive and oxygen-sensitive image contrasts for evaluation of the brain tumor microenvironment. Advantages include fast whole-brain acquisition, in-line B 0 correction, and simultaneous estimation of CEST effects, R 2 , R2*, and R2' at 3 T. © 2018 International Society for Magnetic Resonance in Medicine.

  16. Simultaneous Chronoamperometric Sensing of Ascorbic Acid and Acetaminophen at a Boron-Doped Diamond Electrode

    Directory of Open Access Journals (Sweden)

    Ciprian Radovan

    2008-06-01

    Full Text Available Cyclic voltammetry (CV and chronoamperometry (CA have been used to sense and determine simultaneously L-ascorbic acid (AA and acetaminophen (AC at a boron-doped diamond electrode (BDDE in a Britton-Robinson buffer solution. The calibration plots of anodic current peak versus concentration obtained from CV and CA data for both investigated compounds in single and di-component solutions over the concentration range 0.01 mM – 0.1 mM proved to be linear, with very good correlation parameters. Sensitivity values and RSD of 2-3% were obtained for various situations, involving both individual and simultaneous presence of AA and AC. The chronoamperometric technique associated with standard addition in sequential one step and/or two successive and continuous chronoamperograms at two characteristic potential levels represented a feasible option for the simultaneous determination of AA and AC in real sample systems such as pharmaceutical formulations. The average values indicated by the supplier were confirmed to a very close approximation from chronoamperomgrams by using several additions with the application of suitable current correction factors.

  17. Simultaneous determination of several phytohormones in natural coconut juice by hollow fiber-based liquid-liquid-liquid microextraction-high performance liquid chromatography.

    Science.gov (United States)

    Wu, Yunli; Hu, Bin

    2009-11-06

    A simple, selective, sensitive and inexpensive method of hollow fiber-based liquid-liquid-liquid microextraction (HF-LLLME) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV) detection was developed for the determination of four acidic phytohormones (salicylic acid (SA), indole-3-acetic acid (IAA), (+/-) abscisic acid (ABA) and (+/-) jasmonic acid (JA)) in natural coconut juice. To the best of our knowledge, this is the first report on the use of liquid phase microextraction (LPME) as a sample pretreatment technique for the simultaneous analysis of several phytohormones. Using phenetole to fill the pores of hollow fiber as the organic phase, 0.1molL(-1) NaOH solution in the lumen of hollow fiber as the acceptor phase and 1molL(-1) HCl as the donor phase, a simultaneous preconcentration of four target phytohormones was realized. The acceptor phase was finally withdrawn into the microsyringe and directly injected into HPLC for the separation and quantification of the target phytohormones. The factors affecting the extraction efficiency of four phytohormones by HF-LLLME were optimized with orthogonal design experiment, and the data was analyzed by Statistical Product and Service Solutions (SPSS) software. Under the optimized conditions, the enrichment factors for SA, IAA, ABA and JA were 243, 215, 52 and 48, with the detection limits (S/N=3) of 4.6, 1.3, 0.9ngmL(-1) and 8.8 microg mL(-1), respectively. The relative standard deviations (RSDs, n=7) were 7.9, 4.9, 6.8% at 50ngmL(-1) level for SA, IAA, ABA and 8.4% at 500 microg mL(-1) for JA, respectively. To evaluate the accuracy of the method, the developed method was applied for the simultaneous analysis of several phytohormones in five natural coconut juice samples, and the recoveries for the spiked samples were in the range of 88.3-119.1%.

  18. Simultaneous quantitative detection of multiple tumor markers with a rapid and sensitive multicolor quantum dots based immunochromatographic test strip.

    Science.gov (United States)

    Wang, Chunying; Hou, Fei; Ma, Yicai

    2015-06-15

    A novel multicolor quantum dots (QDs) based immunochromatographic test strip (ICTS) was developed for simultaneous quantitative detection of multiple tumor markers, by utilizing alpha fetoprotein (AFP) and carcinoembryonic antigen (CEA) as models. The immunosensor could realize simultaneous quantitative detection of tumor markers with only one test line and one control line on the nitrocellulose membrane (NC membrane) due to the introduction of multicolor QDs. In this method, a mixture of mouse anti-AFP McAb and mouse anti-CEA McAb was coated on NC membrane as test line and goat anti-mouse IgG antibody was coated as control line. Anti-AFP McAb-QDs546 conjugates and anti-CEA McAb-QDs620 conjugates were mixed and applied to the conjugate pad. Simultaneous quantitative detection of multiple tumor markers was achieved by detecting the fluorescence intensity of captured QDs labels on test line and control line using a test strip reader. Under the optimum conditions, AFP and CEA could be detected as low as 3 ng/mL and 2 ng/mL in 15 min with a sample volume of 80 μL, and no obvious cross-reactivity was observed. The immunosensor was validated with 130 clinical samples and in which it exhibited high sensitivity (93% for AFP and 87% for CEA) and specificity (94% for AFP and 97% for CEA). The immunosensor also demonstrated high recoveries (87.5-113% for AFP and 90-97.3% for CEA) and low relative standard deviations (RSDs) (2.8-6.2% for AFP and 4.9-9.6% for CEA) when testing spiked human serum. This novel multicolor QDs based ICTS provides an easy and rapid, simultaneous quantitative detecting strategy for point-of-care testing of tumor markers. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Simultaneous polarographic determination of micro amounts of vanadium(V) and molybdenum(VI)

    International Nuclear Information System (INIS)

    Rao, V.S.N.; Rao, S.B.

    1979-01-01

    A simple and sensitive polarographic method has been developed for the determination of micro quantities of vanadium(V) and molybdenum(VI), based on the reduction of bromate, which is catalysed by these metal ions in the presence of 2,4-dihydroxyacetophenone oxime. Interference by various cations and anions has been investigated. (author)

  20. Simultaneous and Direct Determination of Vancomycin and Cephalexin in Human Plasma by Using HPLC-DAD Coupled with Second-Order Calibration Algorithms

    Directory of Open Access Journals (Sweden)

    Le-Qian Hu

    2012-01-01

    Full Text Available A simple, rapid, and sensitive method for the simultaneous determination of vancomycin and cephalexin in human plasma was developed by using HPLC-DAD with second-order calibration algorithms. Instead of a completely chromatographic separation, mathematical separation was performed by using two trilinear decomposition algorithms, that is, PARAFAC-alternative least squares (PARAFAC-ALSs and self-weight-alternative-trilinear-decomposition- (SWATLD- coupled high-performance liquid chromatography with DAD detection. The average recoveries attained from PARAFAC-ALS and SWATLD with the factor number of 4 (N=4 were 101±5% and 102±4% for vancomycin, and 96±3% and 97±3% for cephalexininde in real human samples, respectively. The statistical comparison between PARAFAC-ALS and SWATLD is demonstrated to be similar. The results indicated that the combination of HPLC-DAD detection with second-order calibration algorithms is a powerful tool to quantify the analytes of interest from overlapped chromatographic profiles for complex analysis of drugs in plasma.

  1. Simultaneous determination of copper, lead and cadmium by cathodic adsorptive stripping voltammetry using artificial neural network

    International Nuclear Information System (INIS)

    Ensafi, Ali A.; Khayamian, T.; Benvidi, A.; Mirmomtaz, E.

    2006-01-01

    In this work, simultaneous determination of two groups of elements consisting of Pb(II)-Cd(II) and Cu(II)-Pb(II)-Cd(II) using adsorptive cathodic stripping voltammetry are described. The method is based on accumulation of these metal ions on mercury electrode using xylenol orange as a suitable complexing agent. The potential was scanned to the negative direction and the differential pulse stripping voltammograms were recorded. The instrumental and chemical factors were optimized using artificial neural network. The optimized conditions were obtained in pH of 5.5, xylenol orange concentration of 4.0 μM, accumulation potential of -0.50 V, accumulation time of 30 s, scan rate of 10 mV/s and pulse height of 70 mV. The relationship between the peak current versus concentration was linear over the range of 5.0-150.0 ng ml -1 for cadmium and 5.0-150.0 ng ml -1 for lead. The limits of detection were 0.98 and 1.18 ng ml -1 for lead and cadmium ions, respectively. In simultaneous determination of Cu(II), Pb(II) and Cd(II) there are inter-metallic interactions, which result a non-linear relationship between the peak current and the ionic concentration for each of the element. Therefore, an artificial neural network was used as the multivariate calibration method. The ANN was constructed with three neurons as the output layer for the simultaneous determination of the three elements. The constructed model was able to predict the concentration of the elements in the ranges of 1.0-50.0, 5.0-200.0 and 10.0-200.0 ng ml -1 , for Cu(II), Pb(II) and Cd(II), respectively

  2. Self-assembly of graphitic carbon nitride nanosheets–carbon nanotube composite for electrochemical simultaneous determination of catechol and hydroquinone

    International Nuclear Information System (INIS)

    Zhang, Hanqiang; Huang, Yihong; Hu, Shirong; Huang, Qitong; Wei, Chan; Zhang, Wuxiang; Yang, Weize; Dong, Peihui; Hao, Aiyou

    2015-01-01

    Graphical abstract: Schematic diagram of hydrothermal synthesis graphitic carbon nitride nanosheets-carbon nanotube composite and theirs application for electrochemical sensing catechol and hydroquinone. - Highlights: • Self-assembly of graphitic carbon nitride nanosheets-carbon nanotube composite. • CNNS-CNT show more stronger conductivity than CNNS and CNT. • CNNS-CNT has been performed for detection of catechol and hydroquinone. • The probe was applied to detect practical samples with satisfactory results. - Abstract: In this paper, three-dimensional (3D) graphitic carbon nitride nanosheets-carbon nanotube (CNNS-CNT) composite was synthesized via hydrothermal reaction of 2D CNNS and 1D CNT-COOH by π-π stacking and electrostatic interactions. This CNNS-CNT composite was characterized by transmission electron microscope, scanning electron microscope, x-ray diffraction and fourier-transform infrared. In addition, the CNNS-CNT composite displayed excellent conductivity comparing with CNNS and CNT-COOH monomer. This composite was applied for electrochemical simultaneous determination of catechol (CC) and hydroquinone (HQ) with good sensitivity, wide linear range and low detection limit. In addition, this CNNS-CNT composite modified electrode was also applied to detect practical samples with satisfactory results

  3. Sequential Injection Method for Rapid and Simultaneous Determination of 236U, 237Np, and Pu Isotopes in Seawater

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Steier, Peter

    2013-01-01

    An automated analytical method implemented in a novel dual-column tandem sequential injection (SI) system was developed for simultaneous determination of 236U, 237Np, 239Pu, and 240Pu in seawater samples. A combination of TEVA and UTEVA extraction chromatography was exploited to separate and purify...... target analytes, whereupon plutonium and neptunium were simultaneously isolated and purified on TEVA, while uranium was collected on UTEVA. The separation behavior of U, Np, and Pu on TEVA–UTEVA columns was investigated in detail in order to achieve high chemical yields and complete purification...

  4. Eco-friendly ionic liquid assisted capillary electrophoresis and α-acid glycoprotein-assisted liquid chromatography for simultaneous determination of anticancer drugs in human fluids.

    Science.gov (United States)

    Abd El-Hady, Deia; Albishri, Hassan M; Rengarajan, Rajesh

    2015-06-01

    In the current work, two eco-friendly analytical methods based on capillary electrophoresis (CE) and reversed phase liquid chromatography (RPLC) were developed for simultaneous determination of the most commonly used anticancer drugs for Hodgkin's disease: methotrexate (MTX), vinblastine, chlorambucil and dacarbazine. A background electrolyte (BGE) of 12.5 mmol/L phosphate buffer at pH 7.4 and 0.1 µmol/L 1-butyl-3-methyl imidazolium bromide (BMImBr) ionic liquid (IL) was used for CE measurements at 250 nm detection wavelength, 20 kV applied voltage and 25 °C. The rinsing protocol was significantly improved to reduce the adsorption of IL on the interior surface of capillary. Moreover, RPLC method was developed on α-1-acid glycoprotein (AGP) column. Mobile phase was 10 mmol/L phosphate buffer at pH 6.0 (100% v/v) and flow rate at 0.1 mL/min. As AGP is a chiral column, it was successfully separated l-MTX from its enantiomer impurity d-MTX. Good linearity of quantitative analysis was achieved with coefficients of determinations (r(2) ) >0.995. The stability of drugs measurements was investigated with adequate recoveries up to 24 h storage time under ambient temperature. The limits of detection were <50 and 90 ng/mL by CE and RPLC, respectively. The using of short-chain IL as an additive in BGE achieved 600-fold sensitivity enhancement compared with conventional Capillary Zone Electrophoresis (CZE). Therefore, for the first time, the proposed methods were successfully applied to determine simultaneously the analytes in human plasma and urine samples at clinically relevant concentrations with fast and simple pretreatments. Developed IL-assisted CE and RPLC methods were also applied to measure MTX levels in patients' samples over time. Copyright © 2014 John Wiley & Sons, Ltd.

  5. Simultaneous determination of oleanolic acid, ursolic acid, quercetin and apigenin in Swertia mussotii Franch by capillary zone electrophoresis with running buffer modifier.

    Science.gov (United States)

    Gao, Ruibin; Wang, Litao; Yang, Yan; Ni, Jingman; Zhao, Liang; Dong, Shuqing; Guo, Mei

    2015-03-01

    The method of capillary zone electrophoresis (CZE) with direct UV detection was developed for the determination of oleanolic acid, ursolic acid, quercetin and apigenin. and then for the first time successfully applied to the analysis of four analytes in Swertia mussotii Franch and its preparations. Various factors affecting the CZE procedure were investigated and optimized, and the optimal conditions were: 50 × 10(-3) mol/L borate-phosphate buffer (pH 9.5) with 5.0 × 10(-3) mol/L β-cyclodextrin, 15 kV separation voltage, 20 °C column temperature, 250 nm detection wavelength and 5 s electrokinetic injection time (voltage 20 psi). Under the conditions, oleanolic acid, ursolic acid, quercetin and apigenin could be determined within the test ranges with a good correlation coefficient (r(2) > 0.9991). The limits of detection for conditions, oleanolic acid, ursolic acid, quercetin and apigenin were 0.3415, 0.2003, 0.0062 and 0.2538 µg/mL, respectively, and the intra- and inter-day relative standard deviations were no more than 4.72%. This procedure provided a convenient, sensitive and accurate method for simultaneous determination of oleanolic acid, ursolic acid, quercetin and apigenin in S. mussotii Franch. Copyright © 2014 John Wiley & Sons, Ltd.

  6. Sensitivity and specificity of copper sulphate test in determining ...

    African Journals Online (AJOL)

    Background: The accuracy of the copper sulphate method for the rapid screening of prospective blood donors has been questioned because this rapid screening method may lead to false deferral of truly eligible prospective blood donors. Objective: This study was aimed at determining the sensitivity and specificity of copper ...

  7. Highly sensitive determination of mercury using copper enhancer by diamond electrode coupled with sequential injection–anodic stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Chaiyo, Sudkate [Department of Chemistry, Faculty of Science, Srinakharinwirot University (Thailand); Chailapakul, Orawon [Department of Chemistry, Faculty of Science, Chulalongkorn University (Thailand); Center for Petroleum, Petrochemicals, and Advanced Materials, Chulalongkorn University (Thailand); Siangproh, Weena, E-mail: weena@swu.ac.th [Department of Chemistry, Faculty of Science, Srinakharinwirot University (Thailand)

    2014-12-10

    Highlights: • Highly sensitive determination of Hg(II) using SI–ASV-BDD was achieved. • Electrochemical detection of Hg(II) using Cu(II) enhancer was accomplished. • LOD and LOQ were found to be very low at 40.0 ppt and 135.0 ppt. • This method was successfully applied for determination of Hg(II) in real samples. - Abstract: A highly sensitive determination of mercury in the presence of Cu(II) using a boron-doped diamond (BDD) thin film electrode coupled with sequential injection–anodic stripping voltammetry (SI–ASV) was proposed. The Cu(II) was simultaneously deposited with Hg(II) in a 0.5 M HCl supporting electrolyte by electrodeposition. In presence of an excess of Cu(II), the sensitivity for the determination of Hg(II) was remarkably enhanced. Cu(II) and Hg(II) were on-line deposited onto the BDD electrode surface at −1.0 V (vs. Ag/AgCl, 3 M KCl) for 150 s with a flow rate of 14 μL s{sup −1}. An anodic stripping voltammogram was recorded from −0.4 V to 0.25 V using a frequency of 60 Hz, an amplitude of 50 mV, and a step potential of 10 mV at a stopped flow. Under the optimal conditions, well-defined peaks of Cu(II) and Hg(II) were found at −0.25 V and +0.05 V (vs. Ag/AgCl, 3 M KCl), respectively. The detection of Hg(II) showed two linear dynamic ranges (0.1–30.0 ng mL{sup −1} and 5.0–60.0 ng mL{sup −1}). The limit of detection (S/N = 3) obtained from the experiment was found to be 0.04 ng mL{sup −1}. The precision values for 10 replicate determinations were 1.1, 2.1 and 2.9% RSD for 0.5, 10 and 20 ng mL{sup −1}, respectively. The proposed method has been successfully applied for the determination of Hg(II) in seawater, salmon, squid, cockle and seaweed samples. A comparison between the proposed method and an inductively coupled plasma optical emission spectrometry (ICP-OES) standard method was performed on the samples, and the concentrations obtained via both methods were in agreement with the certified values of Hg

  8. Simultaneous determination of psychotropic drugs in human urine by capillary electrophoresis with electrochemiluminescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Li Jianguo [Key Laboratory of Analytical Chemistry for Life Science (Education Ministry of China), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China); School of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215006 (China); Zhao Fengjuan [Key Laboratory of Analytical Chemistry for Life Science (Education Ministry of China), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China); Ju Huangxian [Key Laboratory of Analytical Chemistry for Life Science (Education Ministry of China), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China)]. E-mail: hxju@nju.edu.cn

    2006-08-04

    Amitriptyline, doxepin and chlorpromazine are often used as psychotropic drugs in treatment of the various mental diseases, and are also partly excreted by kidney. This work developed a simple, selective and sensitive method for their simultaneous monitoring in human urine using capillary electrophoresis coupled with electrochemiluminescence (ECL) detection based on end-column ECL reaction of tris-(2,2'-bipyridyl)ruthenium(II) with aliphatic tertiary amino moieties. Acetone was used as an additive to the running buffer to obtain their absolute separation. Under optimized conditions the proposed method displayed a linear range from 5.0 to 800 ng mL{sup -1} for the three drugs with the correlation coefficients more than 0.995 (n = 8). Their limits of detection were 0.8 ng mL{sup -1} (3.6 fg), 1.0 ng mL{sup -1} (4.5 fg) and 1.5 ng mL{sup -1} (6.8 fg) at a signal to noise ratio of 3, respectively. The relative standard deviations for five determinations of 20 ng mL{sup -1} amitriptyline, doxepin and chlorpromazine were 1.7%, 4.2% and 3.6%, respectively. For practical application an extract step with 90:10 heptane/ethyl acetate (v/v) was performed to eliminate the influence of ionic strength in sample. The recoveries of amitriptyline, doxepin and chlorpromazine at different levels in human urine were between 83% and 93%, which showed that the method was valuable in clinical and biochemical laboratories for monitoring amitriptyline, doxepin and chlorpromazine.

  9. Simultaneous gene silencing of Bcl-2, XIAP and Survivin re-sensitizes pancreatic cancer cells towards apoptosis

    International Nuclear Information System (INIS)

    Rückert, Felix; Samm, Nicole; Lehner, Anne-Kathrin; Saeger, Hans-Detlev; Grützmann, Robert; Pilarsky, Christian

    2010-01-01

    Pancreatic ductal adenocarcinoma shows a distinct apoptosis resistance, which contributes significantly to the aggressive nature of this tumor and constrains the effectiveness of new therapeutic strategies. Apoptosis resistance is determined by the net balance of the cells pro-and anti-apoptotic 'control mechanisms'. Numerous dysregulated anti-apoptotic genes have been identified in pancreatic cancer and seem to contribute to the high anti-apoptotic buffering capacity. We aimed to compare the benefit of simultaneous gene silencing (SGS) of several candidate genes with conventional gene silencing of single genes. From literature search we identified the anti-apoptotic genes XIAP, Survivin and Bcl-2 as commonly upregulated in pancreatic cancer. We performed SGS and silencing of single candidate genes using siRNA molecules in two pancreatic cancer cell lines. Effectiveness of SGS was assessed by qRT-PCR and western blotting. Apoptosis induction was measured by flow cytometry and caspase activation. Simultaneous gene silencing reduced expression of the three target genes effectively. Compared to silencing of a single target or control, SGS of these genes resulted in a significant higher induction of apoptosis in pancreatic cancer cells. In the present study we performed a subliminal silencing of different anti-apoptotic target genes simultaneously. Compared to silencing of single target genes, SGS had a significant higher impact on apoptosis induction in pancreatic cancer cells. Thereby, we give further evidence for the concept of an anti-apoptotic buffering capacity of pancreatic cancer cells

  10. Radium 226 and uranium isotopes simultaneously determination in water samples using liquid scintillation counter

    International Nuclear Information System (INIS)

    Al-Masri, M.S.; Al-Akel, B.; Saaid, S.; Nashawati, A.

    2007-04-01

    In this work a method has been developed to determine simultaneously Radium 226 and Uranium isotopes in water samples by low back ground Liquid Scintillation Counter. Radium 226 was determined by its progeny Polonium 214 after one month of sample storage in order to achieve the equilibrium between Radium 226 and Polonium 214. Uranium isotopes were determined by subtracting Radium 226 activity from total alpha activity. The method detection limits were 0.049 Bq/L and 0.176 Bq/L for Radium 226 and Uranium isotopes respectively. The repeatability limits were ± 0.32 Bq/L and ± 0.9 Bq/L for Radium 226 and Uranium isotopes respectively. While relative errors were % 9.5 and %18.2 for Radium 226 and Uranium isotopes respectively. On the other hand, the report presented the results of different standard and natural samples.(author)

  11. Simultaneous determination of chromium(III) and chromium(VI) in aqueous solutions by ion chromatography and chemiluminescence detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jøns, O; Nielsen, B

    1992-01-01

    A method for the simultaneous determination of chromium(iii) and chromium(vi) in a flow system based on chemiluminescence was developed. A Dionex cation-exchange guard column was used to separate chromium(iii) from chromium(vi), and chromium(vi) was reduced by potassium sulfite, whereupon both...

  12. Simultaneous Determination of the Main Peanut Allergens in Foods Using Disposable Amperometric Magnetic Beads-Based Immunosensing Platforms

    Directory of Open Access Journals (Sweden)

    Víctor Ruiz-Valdepeñas Montiel

    2016-06-01

    Full Text Available In this work, a novel magnetic beads (MBs-based immunosensing approach for the rapid and simultaneous determination of the main peanut allergenic proteins (Ara h 1 and Ara h 2 is reported. It involves the use of sandwich-type immunoassays using selective capture and detector antibodies and carboxylic acid-modified magnetic beads (HOOC-MBs. Amperometric detection at −0.20 V was performed using dual screen-printed carbon electrodes (SPdCEs and the H2O2/hydroquinone (HQ system. This methodology exhibits high sensitivity and selectivity for the target proteins providing detection limits of 18.0 and 0.07 ng/mL for Ara h 1 and Ara h 2, respectively, with an assay time of only 2 h. The usefulness of the approach was evaluated by detecting the endogenous content of both allergenic proteins in different food extracts as well as trace amounts of peanut allergen (0.0001% or 1.0 mg/kg in wheat flour spiked samples. The developed platform provides better Low detection limits (LODs in shorter assay times than those claimed for the allergen specific commercial ELISA kits using the same immunoreagents and quantitative information on individual food allergen levels. Moreover, the flexibility of the methodology makes it readily translate to the detection of other food-allergens.

  13. Simultaneous determination of quercetin, kaempferol and isorhamnetin accumulated human breast cancer cells, by high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Yi; Cao, Jiang; Weng, Jian-Hua; Zeng, Su

    2005-09-01

    Quercetin, kaempferol and isorhamnetin are the most important constituents in ginkgo flavonoids. A simple, rapid and sensitive high-performance liquid chromatography method was developed to simultaneously determine quercetin, kaempferol and isorhamnetin absorped by human breast cancer cells. Cells were treated with ginkgo flavonols and then lysed with Triton-X 100. The flavonols in the samples were measured by RP-HPLC with a C18 column after a simple extraction with a mixture of ether and acetone. The mobile phase contained phosphate buffer (pH 2.0; 10 mM) tetrahydrofuran, methanol and isopropanol (65:15:10:20, v/v/v/v). The ultraviolet detector was operated at 380 nm. The calibration curve was linear from 0.1 to 1.0 microM (r > 0.999) for each flavonol. The mean extraction efficiency was about 70%. The recovery of the assay was between 98.9 and 100.6%. The limit of detection was 0.01 microM for quercetin and kaempferol and 0.05 microM for isorhamnetin. The limit of quantitation was 0.1 microM (R.S.D.method was applied to quantify quercetin, kaempferol and isorhamnetin in human breast cancer Bcap37 and Bcap37/MDR1 cells.

  14. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Xing Zhi [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Kuermaiti, Biekesailike [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Products Quality Inspection Institute, Yili, Xinjiang 835000 (China); Wang Juan; Han Guojun; Zhang Sichun [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Zhang Xinrong, E-mail: xrzhang@mail.tsinghua.edu.cn [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China)

    2010-12-15

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 {mu}g L{sup -1}, respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  15. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    International Nuclear Information System (INIS)

    Xing Zhi; Kuermaiti, Biekesailike; Wang Juan; Han Guojun; Zhang Sichun; Zhang Xinrong

    2010-01-01

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 μg L -1 , respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  16. Validated Spectrophotometric Methods for Simultaneous Determination of Food Colorants and Sweeteners

    Directory of Open Access Journals (Sweden)

    Fatma Turak

    2013-01-01

    Full Text Available Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue and two sweeteners (Acesulfame-K and Aspartame in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS, is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K and third-derivative curve (for Aspartame and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS, depends on application ratio spectra of first- and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992–0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 μgmL−1 and from 0.06 to 0.47 μgmL−1, respectively. The intraday and interday precision tests produced good RSD% values (<0.81%; recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.

  17. Simultaneous determination of 18 pyrethroids in indoor air by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Yoshida, Toshiaki

    2009-06-26

    An analytical method was developed for the simultaneous measurement of 18 pyrethroids (allethrin, bifenthrin, cyfluthrin, cypermethrin, cyphenothrin, deltamethrin, empenthrin, fenpropathrin, furamethrin, imiprothrin, metofluthrin, permethrin, phenothrin, prallethrin, profluthrin, resmethrin, tetramethrin and transfluthrin) in indoor air. The pyrethroids were collected for 24 h using a combination of adsorbents (quartz fiber filter disk and Empore C18 disk), with protection from light, and then extracted with acetone, concentrated, and analyzed by GC/MS. They could be determined accurately and precisely (detection limits: ca. 1 ng/m(3)). The collected pyrethroid samples could be stored for up to one month at 4 degrees C in a refrigerator.

  18. Simultaneous determination of CRP and D-dimer in human blood plasma samples with White Light Reflectance Spectroscopy.

    Science.gov (United States)

    Koukouvinos, Georgios; Petrou, Panagiota; Misiakos, Konstantinos; Drygiannakis, Dimitris; Raptis, Ioannis; Stefanitsis, Gerasimos; Martini, Spyridoula; Nikita, Dimitra; Goustouridis, Dimitrios; Moser, Isabella; Jobst, Gerhard; Kakabakos, Sotirios

    2016-10-15

    A dual-analyte assay for the simultaneous determination of C-reactive protein (CRP) and D-dimer in human blood plasma based on a white light interference spectroscopy sensing platform is presented. Measurement is accomplished in real-time by scanning the sensing surface, on which distinct antibody areas have been created, with a reflection probe used both for illumination of the surface and collection of the reflected interference spectrum. The composition of the transducer, the sensing surface chemical activation and biofunctionalization procedures were optimized with respect to signal magnitude and repeatability. The assay format involved direct detection of CRP whereas for D-dimer a two-site immunoassay employing a biotinylated reporter antibody and reaction with streptavidin was selected. The assays were sensitive with detection limits of 25ng/mL for both analytes, precise with intra- and inter-assay CV values ranging from 3.6% to 7.7%, and from 4.8% to 9.5%, respectively, for both assays, and accurate with recovery values ranging from 88.5% to 108% for both analytes. Moreover, the values determined for the two analytes in 35 human plasma samples were in excellent agreement with those received for the same samples by standard diagnostic laboratory instrumentation employing commercial kits. The excellent agreement of the results supported the validity of the proposed system for clinical application for the detection of multiple analytes since it was demonstrated that up to seven antibody areas can be created on the sensing surface and successfully interrogated with the developed optical set-up. Copyright © 2015. Published by Elsevier B.V.

  19. Simultaneous Determination of Parathion, Malathion, Diazinon, and Pirimiphos Methyl in Dried Medicinal Plants Using Solid-Phase Microextraction Fibre Coated with Single-Walled Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Reza Ahmadkhaniha

    2012-01-01

    Full Text Available A reliable and sensitive headspace solid-phase microextraction gas chromatography-mass spectrometry method for simultaneous determination of different organophosphorus pesticides in dried medicinal plant samples is described. The analytes were extracted by single-walled carbon nanotubes as a new solid-phase microextraction adsorbent. The developed method showed good performance. For diazinon and pirimiphos methyl calibration, curves were linear (r2≥0.993 over the concentration ranges from 1.5 to 300 ng g−1, and the limit of detection at signal-to-noise ratio of 3 was 0.3 ng g−1. For parathion and malathion, the linear range and limit of detection were 2.5–300 (r2≥0.991 and 0.5 ng g−1, respectively. In addition, a comparative study between the single-walled carbon nanotubes and a commercial polydimethylsiloxane fibre for the determination of target analytes was carried out. Single-walled carbon nanotubes fibre showed higher extraction capacity, better thermal stability (over 350∘C, and longer lifespan (over 250 times than the commercial polydimethylsiloxane fibre. The developed method was successfully applied to determine target organophosphorus pesticides in real samples.

  20. Simultaneous Voltammetric Determination of Acetaminophen and Isoniazid (Hepatotoxicity-Related Drugs) Utilizing Bismuth Oxide Nanorod Modified Screen-Printed Electrochemical Sensing Platforms.

    Science.gov (United States)

    Mahmoud, Bahaa G; Khairy, Mohamed; Rashwan, Farouk A; Banks, Craig E

    2017-02-07

    To overcome the recent outbreaks of hepatotoxicity-related drugs, a new analytical tool for the continuously determination of these drugs in human fluids is required. Electrochemical-based analytical methods offer an effective, rapid, and simple tool for on-site determination of various organic and inorganic species. However, the design of a sensitive, selective, stable, and reproducible sensor is still a major challenge. In the present manuscript, a facile, one-pot hydrothermal synthesis of bismuth oxide (Bi 2 O 2.33 ) nanostructures (nanorods) was developed. These BiO nanorods were cast onto mass disposable graphite screen-printed electrodes (BiO-SPEs), allowing the ultrasensitive determination of acetaminophen (APAP) in the presence of its common interference isoniazid (INH), which are both found in drug samples. The simultaneous electroanalytical sensing using BiO-SPEs exhibited strong electrocatalytic activity toward the sensing of APAP and INH with an enhanced analytical signal (voltammetric peak) over that achievable at unmodified (bare) SPEs. The electroanalytical sensing of APAP and INH are possible with accessible linear ranges from 0.5 to 1250 μM and 5 to 1760 μM with limits of detection (3σ) of 30 nM and 1.85 μM, respectively. The stability, reproducibility, and repeatability of BiO-SPE were also investigated. The BiO-SPEs were evaluated toward the sensing of APAP and INH in human serum, urine, saliva, and tablet samples. The results presented in this paper demonstrate that BiO-SPEs sensing platforms provide a potential candidate for the accurate determination of APAP and INH within human fluids and pharmaceutical formulations.

  1. Antioxidant activity of leaf extracts from different Hibiscus sabdariffa accessions and simultaneous determination five major antioxidant compounds by LC-Q-TOF-MS.

    Science.gov (United States)

    Wang, Jin; Cao, Xianshuang; Jiang, Hao; Qi, Yadong; Chin, Kit L; Yue, Yongde

    2014-12-17

    Hibiscus sabdariffa has gained attention for its antioxidant activity. There are many accessions of H. sabdariffa in the world. However, information on the quantification of antioxidant compounds in different accessions is rather limited. In this paper, a liquid chromatography/quadrupole-time-of-flight mass spectrometry (LC-Q-TOF-MS) method for simultaneous determination of five antioxidant compounds (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, and isoquercitrin) in H. sabdariffa leaves was developed. The method was validated for linearity, sensitivity, precision, repeatability and accuracy. The validated method has been successfully applied for determination of the five analytes in eight accessions of H. sabdariffa. The eight accessions of H. sabdariffa were evaluated for their antioxidant activities by DPPH free radical scavenging assay. The investigated accessions of H. sabdariffa were rich in rutin and exhibited strong antioxidant activity. The two accessions showing the highest antioxidant activities were from Cuba (No. 2) and Taiwan (No. 5). The results indicated that H. sabdariffa leaves could be considered as a potential antioxidant source for the food industry. The developed LC-Q-TOF-MS method is helpful for quality control of H. sabdariffa.

  2. Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk.

    Science.gov (United States)

    Hou, Xiao-Lin; Chen, Guo; Zhu, Li; Yang, Ting; Zhao, Jian; Wang, Lei; Wu, Yin-Liang

    2014-07-01

    A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 38 veterinary drugs (18 sulfonamides, 11 quinolones and 9 benzimidazoles) and 8 metabolites of benzimidazoles in bovine milk by ultra high performance liquid chromatography-positive electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Samples were extracted with acidified acetonitrile, cleaned up with Oasis(®) MCX cartridges, and analyzed by LC-MS/MS on an Acquity UPLC(®) BEH C18 column with gradient elution. The method allows such multi-analyte measurements within a 13min runtime while the specificity is ensured through the MRM acquisition mode. The method was validated according to the European Commission Decision 2002/657/EC determining specificity, decision limit (CCα), detection capability (CCβ), recovery, precision, linearity and stability. For compounds which have MRLs in bovine milk, the CCα values fall into a range from 11 to 115μg/kg, and the CCβ values fall within a range of 12-125μg/kg. For compounds which have not MRLs in bovine milk, the CCα values fall into a range from 0.01 to 0.08μg/kg, and the CCβ values fall within a range of 0.02-0.11μg/kg. The mean recoveries of the 46 analytes were between 87 and 119%. The calculated RSD values of repeatability and within-laboratory reproducibility experiments were below 11% and 15% for the 46 compounds, respectively. The method was demonstrated to be suitable for the simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Simultaneous determination of two active components of pharmaceutical preparations by sequential injection method using heteropoly complexes

    Directory of Open Access Journals (Sweden)

    Mohammed Khair E. A. Al-Shwaiyat

    2014-12-01

    Full Text Available New approach has been proposed for the simultaneous determination of two reducing agents based on the dependence of their reaction rate with 18-molybdo-2-phosphate heteropoly complex on pH. The method was automated using the manifold typical for the sequential analysis method. Ascorbic acid and rutin were determined by successive injection of two samples acidified to different pH. The linear range for rutin determination was 0.6-20 mg/L and the detection limit was 0.2 mg/L (l = 1 cm. The determination of rutin was possible in the presence of up to a 20-fold excess of ascorbic acid. The method was successfully applied to the determination of ascorbic acid and rutin in ascorutin tablets. The applicability of the proposed method for the determination of total polyphenol content in natural plant samples was shown.

  4. Simultaneous Determination of Ciprofloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Eye Drops by HPLC

    OpenAIRE

    Katakam, Prakash; Sireesha, Karanam R.

    2012-01-01

    A liquid chromatographic method was developed and validated for the simultaneous determination of ciprofloxacin hydrochloride and dexamethasone sodium phosphate in bulk and pharmaceutical formulations. Optimum separation was achieved in less than 5 min using a C18 column (250 mmx4.6 mm i.d, 5μ particle size) by isocratic elution. The mobile phase consisting of a mixture of mixed phosphate buffer (pH 4) and acetonitrile (65:35, v/v) was used. Column effluents were monitored at 254 nm at a flow...

  5. Simultaneous determination of aliphatic hydrocarbons, PCBs and PCTs in pork liver by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez-Barros, C [Dept. de Quimica Analitica, Nutricion y Bromatologia, Area Nutricion y Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Alvarez Pineiro, M E [Inst. de Investigacion y Analisis Alimentarios, Lab. de Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Simal Lozano, J [Dept. de Quimica Analitica, Nutricion y Bromatologia, Area Nutricion y Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Lage Yusty, M A [Inst. de Investigacion y Analisis Alimentarios, Lab. de Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain)

    1996-10-01

    A multicomponent extraction/concentration procedure has been developed for the enrichment of PCBs, PCTs and aliphatic hydrocarbons (pristane, C{sub 18}, C{sub 19}, C{sub 20}, C{sub 22}, C{sub 24}, C{sub 28}, C{sub 32} and C{sub 36}) in pork liver. These components of the enriched extract were then simultaneously determined by gas chromatography. Mean recoveries ranged from 81.5% for pristane to 93% for PCBs; CV % (0.9-6.7) indicated the method to be both precise and reproducible. (orig.)

  6. Simultaneous determination of nitrogen and phosphorus in cereals using 14 MeV Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Bejarano, R.

    1992-01-01

    A method using 14 MeV neutron activation analysis was developed form non-destructive simultaneous determination of N and P in cereals. The samples were irradiated 5 min. after 0,5 min. decay time. The induced activities were measured using gamma spectrometry with Nal(Tl) well type detector. The accuracy, precision and detection limits obtained are discussed as well as the analytical results for different types of cereals. (Author) 10 refs., 8 tab., 1 fig

  7. Simultaneous determination of low-molecular-weight organic acids and chlorinated acid herbicides in environmental water by a portable CE system with contactless conductivity detection.

    Science.gov (United States)

    Xu, Yan; Wang, Weilong; Li, Sam Fong Yau

    2007-05-01

    This report describes a method to simultaneously determine 11 low-molecular-weight (LMW) organic acids and 16 chlorinated acid herbicides within a single run by a portable CE system with contactless conductivity detection (CCD) in a poly(vinyl alcohol) (PVA)-coated capillary. Under the optimized condition, the LODs of CE-CCD ranged from 0.056 to 0.270 ppm, which were better than for indirect UV (IUV) detection of the 11 LMW organic acids or UV detection of the 16 chlorinated acid herbicides. Combined with an on-line field-amplified sample stacking (FASS) procedure, sensitivity enhancement of 632- to 1078-fold was achieved, with satisfactory reproducibility (RSDs of migration times less than 2.2%, and RSDs of peak areas less than 5.1%). The FASS-CE-CCD method was successfully applied to determine the two groups of acidic pollutants in two kinds of environmental water samples. The portable CE-CCD system shows advantages such as simplicity, cost effectiveness, and miniaturization. Therefore, the method presented in this report has great potential for onsite analysis of various pollutants at the trace level.

  8. Sensitive simultaneous detection of seven sexually transmitted agents in semen by multiplex-PCR and of HPV by single PCR.

    Directory of Open Access Journals (Sweden)

    Fabrícia Gimenes

    Full Text Available Sexually transmitted diseases (STDs may impair sperm parameters and functions thereby promoting male infertility. To date limited molecular studies were conducted to evaluate the frequency and type of such infections in semen Thus, we aimed at conceiving and validating a multiplex PCR (M-PCR assay for the simultaneous detection of the following STD pathogens in semen: Chlamydia trachomatis, Neisseria gonorrhoeae, Mycoplasma genitalium, Trichomonas vaginalis, Herpes virus simplex (HSV -1 and -2, and Treponema pallidum; We also investigated the potential usefulness of this M-PCR assay in screening programs for semen pathogens. In addition, we aimed: to detect human Papillomavirus (HPV and genotypes by single PCR (sPCR in the same semen samples; to determine the prevalence of the seven STDs, HPV and co-infections; to assess the possibility that these infections affect semen parameters and thus fertility. The overall validation parameters of M-PCR were extremely high including agreement (99.2%, sensitivity (100.00%, specificity (99.70%, positive (96.40% and negative predictive values (100.00% and accuracy (99.80%. The prevalence of STDs was very high (55.3%. Furthermore, associations were observed between STDs and changes in semen parameters, highlighting the importance of STD detection in semen. Thus, this M-PCR assay has great potential for application in semen screening programs for pathogens in infertility and STD clinics and in sperm banks.

  9. Simultaneous determination of eight water-soluble vitamins in supplemented foods by liquid chromatography.

    Science.gov (United States)

    Zafra-Gómez, Alberto; Garballo, Antonio; Morales, Juan C; García-Ayuso, Luis E

    2006-06-28

    A fast, simple, and reliable method for the isolation and determination of the vitamins thiamin, riboflavin, niacin, pantothenic acid, pyridoxine, folic acid, cyanocobalamin, and ascorbic acid in food samples is proposed. The most relevant advantages of the proposed method are the simultaneous determination of the eight more common vitamins in enriched food products and a reduction of the time required for quantitative extraction, because the method consists merely of the addition of a precipitation solution and centrifugation of the sample. Furthermore, this method saves a substantial amount of reagents as compared with official methods, and minimal sample manipulation is achieved due to the few steps required. The chromatographic separation is carried out on a reverse phase C18 column, and the vitamins are detected at different wavelengths by either fluorescence or UV-visible detection. The proposed method was applied to the determination of water-soluble vitamins in supplemented milk, infant nutrition products, and milk powder certified reference material (CRM 421, BCR) with recoveries ranging from 90 to 100%.

  10. Simultaneous determination of 19 flavonoids in commercial trollflowers by using high-performance liquid chromatography and classification of samples by hierarchical clustering analysis.

    Science.gov (United States)

    Song, Zhiling; Hashi, Yuki; Sun, Hongyang; Liang, Yi; Lan, Yuexiang; Wang, Hong; Chen, Shizhong

    2013-12-01

    The flowers of Trollius species, named Jin Lianhua in Chinese, are widely used traditional Chinese herbs with vital biological activity that has been used for several decades in China to treat upper respiratory infections, pharyngitis, tonsillitis, and bronchitis. We developed a rapid and reliable method for simultaneous quantitative analysis of 19 flavonoids in trollflowers by using high-performance liquid chromatography (HPLC). Chromatography was performed on Inertsil ODS-3 C18 column, with gradient elution methanol-acetonitrile-water with 0.02% (v/v) formic acid. Content determination was used to evaluate the quality of commercial trollflowers from different regions in China, while three Trollius species (Trollius chinensis Bunge, Trollius ledebouri Reichb, Trollius buddae Schipcz) were explicitly distinguished by using hierarchical clustering analysis. The linearity, precision, accuracy, limit of detection, and limit of quantification were validated for the quantification method, which proved sensitive, accurate and reproducible indicating that the proposed approach was applicable for the routine analysis and quality control of trollflowers. © 2013.

  11. Simultaneous Determination of Florfenicol and Diclazuril in Compound Powder by RP-HPLC-UV Method

    Directory of Open Access Journals (Sweden)

    Leilei Guo

    2014-01-01

    Full Text Available A RP-HPLC-UV method was developed and validated for simultaneous determination of florfenicol and diclazuril in compound powder. The separation involved using a SinoChoom ODS-BP C18 (5 μm, 4.6 mm × 250 mm analytical column. The mobile phase was a mixture of acetonitrile-0.2% phosphoric acid (pH was adjusted to 3.0 with triethylamine. The ratio of acetonitrile and 0.2% phosphoric acid in the mobile phase was 60 : 40 (v/v from 0 minutes to 6 minutes and 70 : 30 (v/v from 6.1 minutes to 15 minutes. The flow rate was 1 mL/min. The temperature of the analytical column was maintained at 30°C. The detection was monitored at 225 nm and 277 nm for florfenicol and diclazuril, respectively. The excipients in the compound powder did not interfere with the drug peaks. The calibration curves of florfenicol and diclazuril were fairly linear over the concentration ranges between 50.0–500.0 μg/mL (r=0.9995 and 10.0–100.0 μg/mL (r=0.9992, respectively. The RSD of both the intraday and interday variations was below 2.1% for florfenicol and diclazuril. The method was successfully validated according to International Conference on Harmonisation and proved to be suitable for the simultaneous determination of florfenicol and diclazuril in compound powder.

  12. Fabrication and application of a new modified electrochemical sensor using nano-silica and a newly synthesized Schiff base for simultaneous determination of Cd{sup 2+}, Cu{sup 2+} and Hg{sup 2+} ions in water and some foodstuff samples

    Energy Technology Data Exchange (ETDEWEB)

    Afkhami, Abbas, E-mail: afkhami@basu.ac.ir [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Soltani-Felehgari, Farzaneh; Madrakian, Tayyebeh; Ghaedi, Hamed [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Rezaeivala, Majid [Department of Chemical Engineering, Hamedan University of Technology, Hamedan (Iran, Islamic Republic of)

    2013-04-10

    Highlights: ► A new modified electrochemical sensor was constructed and used. ► A new Schiff base coated nano-silica was used as modifier. ► The electrochemical properties of electrode were studied. ► This modifier enhanced the electrochemical properties of electrode. ► The electrode was used for simultaneous determination of Cd{sup 2+}, Cu{sup 2+} and Hg{sup 2+} ions. -- Abstract: A new chemically modified carbon paste electrode was constructed and used for rapid, simple, accurate, selective and highly sensitive simultaneous determination of cadmium, copper and mercury using square wave anodic stripping voltammetry (SWASV). The carbon paste electrode was modified by N,N′-bis(3-(2-thenylidenimino)propyl)piperazine coated silica nanoparticles. Compared with carbon paste electrode, the stripping peak currents had a significant increase at the modified electrode. Under the optimized conditions (deposition potential, −1.100 V vs. Ag/AgCl; deposition time, 60 s; resting time, 10 s; SW frequency, 25 Hz; pulse amplitude, 0.15 V; dc voltage step height, 4.4 mV), the detection limit was 0.3, 0.1 and 0.05 ng mL{sup −1} for the determination of Cd{sup 2+}, Cu{sup 2+} and Hg{sup 2+}, respectively. The complexation reaction of the ligand with several metal cations in methanol was studied and the stability constants of the complexes were obtained. The effects of different cations and anions on the simultaneous determination of metal ions were studied and it was found that the electrode is highly selective for the simultaneous determination of Cd{sup 2+}, Cu{sup 2+} and Hg{sup 2+}. Furthermore, the present method was applied to the determination of Cd{sup 2+}, Cu{sup 2+} and Hg{sup 2+} in water and some foodstuff samples.

  13. Simultaneous determination of levocetirizine and pseudoephedrine in dog plasma by liquid chromatography-mass spectrometry in the presence of dextrocetirizine.

    Science.gov (United States)

    Ryu, Jae Kuk; Yoo, Sun Dong

    2012-01-01

    This study describes the development of a rapid and sensitive LC-ESI-MS assay for simultaneous enantioselective determination of levocetirizine and pseudoephedrine in dog plasma in the presence of dextrocetirizine. Separations were achieved on an Ultron ES-OVM chiral column using the mobile phase consisting of 10 mM aqueous NH4OAc (pH 6.6) and acetonitrile (9:1 v/v). The retention times of pseudoephedrine, dextrocetirizine, levocetirizine and diazepam (internal standard) were 5.2, 8.3, 9.6 and 11.6 min, respectively, and the total run time was less than 15 min. The assay was validated to demonstrate the linearity, accuracy and precision, recovery and stability. The calibration curves were linear over the concentration range from 1 - 200 ng/mL for levocetirizine and from 5 - 1000 ng/mL for pseudoephedrine. The developed assay was successfully applied to a pharmacokinetic study after oral administration of the racemic cetirizine (0.5 mg/kg, or 0.25 mg/kg as levocetirizine) and pseudoephedrine (12 mg/kg) in the dog. This article is open to POST-PUBLICATION REVIEW. Registered readers (see "For Readers") may comment by clicking on ABSTRACT on the issue's contents page.

  14. Immunoglobulin E sensitization to cross-reactive carbohydrate determinants: epidemiological study of clinical relevance and role of alcohol consumption

    DEFF Research Database (Denmark)

    Linneberg, Allan; Fenger, Runa Vavia; Husemoen, Lise-Lotte

    2010-01-01

    The determinants and biologic significance of IgE-mediated sensitization to cross-reactive carbohydrate determinants (CCDs) are not entirely known. An association between alcohol consumption and CCD sensitization has been reported in studies from Spain and Portugal.......The determinants and biologic significance of IgE-mediated sensitization to cross-reactive carbohydrate determinants (CCDs) are not entirely known. An association between alcohol consumption and CCD sensitization has been reported in studies from Spain and Portugal....

  15. New method for simultaneous determination of 55Fe and 59Fe in blood serum samples

    International Nuclear Information System (INIS)

    Saukkonen, H.; Uhlenius, R.

    1978-01-01

    Routine methods for the measurement of 55 Fe and 59 Fe activities in biological samples are frequently required in metabolic studies of iron. A new simple method for the simultaneous determination of 59 Fe and 55 Fe concentration in 5 cm 3 samples of blood is described and carefully evaluated. Before the measurement of the activity, organic matter was eliminated by HNO 3 -HClO 4 wet ashing and iron was electroplated onto a copper plate. The accuracy of results was studied by assessing samples, which contained known amounts of radioactivity and determining the counts per nanocurie in each case. The accuracy of the results of 59 Fe and 55 Fe determinations was found to be about 5%. The method has been routinely used to determine iron resorption in patients using the double isotope method. The determination proved to be satisfactory and not too laborious. When performing the yield determination there is a way of detecting and correcting mistakes or incompleteness in different stages of the measurement, thus leading to a high degree of reliability. (T.G.)

  16. Polymeric microchip for the simultaneous determination of anions and cations by hydrodynamic injection using a dual-channel sequential injection microchip electrophoresis system.

    Science.gov (United States)

    Gaudry, Adam J; Nai, Yi Heng; Guijt, Rosanne M; Breadmore, Michael C

    2014-04-01

    A dual-channel sequential injection microchip capillary electrophoresis system with pressure-driven injection is demonstrated for simultaneous separations of anions and cations from a single sample. The poly(methyl methacrylate) (PMMA) microchips feature integral in-plane contactless conductivity detection electrodes. A novel, hydrodynamic "split-injection" method utilizes background electrolyte (BGE) sheathing to gate the sample flows, while control over the injection volume is achieved by balancing hydrodynamic resistances using external hydrodynamic resistors. Injection is realized by a unique flow-through interface, allowing for automated, continuous sampling for sequential injection analysis by microchip electrophoresis. The developed system was very robust, with individual microchips used for up to 2000 analyses with lifetimes limited by irreversible blockages of the microchannels. The unique dual-channel geometry was demonstrated by the simultaneous separation of three cations and three anions in individual microchannels in under 40 s with limits of detection (LODs) ranging from 1.5 to 24 μM. From a series of 100 sequential injections the %RSDs were determined for every fifth run, resulting in %RSDs for migration times that ranged from 0.3 to 0.7 (n = 20) and 2.3 to 4.5 for peak area (n = 20). This system offers low LODs and a high degree of reproducibility and robustness while the hydrodynamic injection eliminates electrokinetic bias during injection, making it attractive for a wide range of rapid, sensitive, and quantitative online analytical applications.

  17. Simultaneous and rapid determination of multiple component concentrations in a Kraft liquor process stream

    Science.gov (United States)

    Li, Jian [Marietta, GA; Chai, Xin Sheng [Atlanta, GA; Zhu, Junyoung [Marietta, GA

    2008-06-24

    The present invention is a rapid method of determining the concentration of the major components in a chemical stream. The present invention is also a simple, low cost, device of determining the in-situ concentration of the major components in a chemical stream. In particular, the present invention provides a useful method for simultaneously determining the concentrations of sodium hydroxide, sodium sulfide and sodium carbonate in aqueous kraft pulping liquors through use of an attenuated total reflectance (ATR) tunnel flow cell or optical probe capable of producing a ultraviolet absorbency spectrum over a wavelength of 190 to 300 nm. In addition, the present invention eliminates the need for manual sampling and dilution previously required to generate analyzable samples. The inventive method can be used in Kraft pulping operations to control white liquor causticizing efficiency, sulfate reduction efficiency in green liquor, oxidation efficiency for oxidized white liquor and the active and effective alkali charge to kraft pulping operations.

  18. A glassy carbon electrode modified with an amphiphilic, electroactive and photosensitive polymer and with multi-walled carbon nanotubes for simultaneous determination of dopamine and paracetamole

    International Nuclear Information System (INIS)

    Liu, Ren; Zeng, Xuebiao; Liu, Jingcheng; Luo, Jing; Zheng, Yuanyi; Liu, Xiaoya

    2016-01-01

    The article describes an electrochemical sensor for simultaneous determination of dopamine (DA) and paracetamole (PAT). It is based on the use of an electroactive polymer (referred to as BPVCM) to functionalize multi-walled carbon nanotubes. BPVCM is a branched amphiphilic photo-sensitive and electroactive polymer that was obtained by copolymerization of a vinyl benzyl carbazole, maleic acid anhydride, 4-vinyl benzylthiol and a vinylbenzyl oxycoumarin. BPVCM efficiently disperses MWCNT in aqueous solution. The electropolymerization of the carbazole moieties of the BPVCM enhances the current response. It also facilitates electron transfer in the MWCNT-BPVCM hybrid as evidenced by cyclic voltammetry and electrochemical impedance spectroscopy. A glassy carbon electrode modified with the nanocomposite displays outstanding electrocatalytic activity towards DA and PAT. DA can be determined, best at a working voltage of 0.2 V (vs. SCE), in the 5 to 1000 μM concentration range with a 2.3 μM detection limit. PAT can be determined in parallel, at a working voltage of 0.39 V (vs. SCE), in the same concentration range with a 3.5 μM detection limit. This analytical range of this method is wider than that of most alternative methods. (author)

  19. New synthesis of poly ortho-methoxyaniline nanostructures and its application to construct modified multi-wall carbon nanotube/graphite paste electrode for simultaneous determination of uric acid and folic acid

    Energy Technology Data Exchange (ETDEWEB)

    Rajabi, Hossein, E-mail: h.rajabi8086@gmail.com; Noroozifar, Meissam

    2017-06-01

    Uric acid (UA) and folic acid (FA) are compounds of biomedical interest. In humans, about 70% of daily uric acid disposal occurs via the kidneys, and in 5–25% of humans, impaired renal (kidney) excretion leads to hyperuricemia. Folate is another form folic acid of which is known as, is one of the B vitamins. It is used as a supplement by women to prevent neural tube defects developing during pregnancy. Polyortho-methoxyaniline nanostructures (POMANS) was synthesized with a new two phase (organic-water) synthesis method. The POMANS was characterized using transmission electron microscopy (TEM) and Fourier transform IR (FTIR). This polymer was used to construct a modified multi-wall carbon nanotube, graphite paste electrode (POMANS-MWCNT/GPE). Linear sweep voltammograms (LSV), cyclic voltammetry (CV) and chronoamperometry were used to investigate the suitability of polyortho-methoxyaniline with multi-wall carbon nanotubes paste electrode as a modifier for the electrocatalytic oxidation of UA and FA in aqueous solutions with various pHs. The results showed that POMANS-MWCNT/GPE had high anodic peak currents for the electrooxidation of UA and FA in pH 6.0.Under the optimized conditions, The catalytic peak currents obtained, was linearly dependent on the UA and FA concentrations in the range of 0.6–52 and 0.5–68 μM with two segments and the detection limits 0.157 and 0.113 μM for UA and FA were, respectively. Finally, the proposed method was also examined as a sensitive, simple and inexpensive electrochemical sensor for the simultaneous determination of UA and FA in real samples such as urine and serum. - Highlights: • For the first time, POMANS was synthesized with a new method of two-phase organic & water. • POMANS-MWCNT/GPE was used for simultaneous determination of UA and FA at optimum pH 6.0. • Parameters n and α were also determined for UA and FA. • Electrochemical simultaneous determination of UA and FA with modified electrode real samples.

  20. Simultaneous determination of 20 components in red wine by LC-MS: application to variations of red wine components in decanting.

    Science.gov (United States)

    Cui, Yan; Li, Qing; Liu, Zhenzhen; Geng, Lulu; Zhao, Xu; Chen, Xiaohui; Bi, Kaishun

    2012-11-01

    The decanting of red wines has a long tradition in red wine service from the perspective of modifying the aroma or taste of a wine. A simple and sensitive liquid chromatography-mass spectrometry method was developed for the simultaneous determination of 20 organic acids and polyphenols in decanting red wine. The separation was performed on a Diamonsil C(18) column (250 mm × 4.6 mm, 5 μm) using a mobile phase composed of methanol-0.1% acetic acid under gradient elution. Analysis was performed in selected ion monitoring mode with negative electrospray ionization interface. All the linear regressions showed good linear relationships (r(2) > 0.9973) between the peak area and concentration of each marker. The assay was reproducible with overall intra and interday variation of less than 5.0%. The recoveries for the quantified compounds were observed over the range of 92.1-108.3% with RSD values less than 5.7%. The method developed was successfully applied to determine the variations of the 20 components in red wine after decanting in different conditions. Concentrations of most organic acids and polyphenols investigated in the red wine were decreased in decanting. In addition, increment of duration, temperature, and light intensity would intensify the changes. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Composite of Cu metal nanoparticles-multiwall carbon nanotubes-reduced graphene oxide as a novel and high performance platform of the electrochemical sensor for simultaneous determination of nitrite and nitrate

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Hasan, E-mail: h.bagheri@bmsu.ac.ir [Chemical Injuries Research Center, Baqiyatallah University of Medical Sciences, Tehran (Iran, Islamic Republic of); Hajian, Ali [Laboratory for Sensors, Department of Microsystems Engineering (IMTEK), University of Freiburg, Georges Köhler Allee 103, 79110 Freiburg (Germany); Rezaei, Mosayeb; Shirzadmehr, Ali [Young Researchers and Elite Club, Hamedan Branch, Islamic Azad University, Hamedan (Iran, Islamic Republic of)

    2017-02-15

    Highlights: • An electrochemical sensor based on Cu metal nanoparticles-multiwall carbon nanotubes-reduced graphene oxide modified glassy carbon electrode was developed. • Simultaneous electrochemical determination of nitrate and nitrite by fabricated sensor was performed. • Modification improved the sensitivity and detection limit of the method. • It is a useful method for determining of nitrate and nitrite in various real samples. - Abstract: In the present research, we aimed to fabricate a novel electrochemical sensor based on Cu metal nanoparticles on the multiwall carbon nanotubes-reduced graphene oxide nanosheets (Cu/MWCNT/RGO) for individual and simultaneous determination of nitrite and nitrate ions. The morphology of the prepared nanocomposite on the surface of glassy carbon electrode (GCE) was characterized using various methods including scanning electron microscopy (SEM), atomic force microscopy (AFM), and electrochemical impedance spectroscopy. Under optimal experimental conditions, the modified GCE showed excellent catalytic activity toward the electro-reduction of nitrite and nitrate ions (pH = 3.0) with a significant increase in cathodic peak currents in comparison with the unmodified GCE. By square wave voltammetry (SWV) the fabricated sensor demonstrated wide dynamic concentration ranges from 0.1 to 75 μM with detection limits (3S{sub b}/m) of 30 nM and 20 nM method for nitrite and nitrate ions, respectively. Furthermore, the applicability of the proposed modified electrode was demonstrated by measuring the concentration of nitrite and nitrate ions in the tap and mineral waters, sausages, salami, and cheese samples.

  2. Composite of Cu metal nanoparticles-multiwall carbon nanotubes-reduced graphene oxide as a novel and high performance platform of the electrochemical sensor for simultaneous determination of nitrite and nitrate

    International Nuclear Information System (INIS)

    Bagheri, Hasan; Hajian, Ali; Rezaei, Mosayeb; Shirzadmehr, Ali

    2017-01-01

    Highlights: • An electrochemical sensor based on Cu metal nanoparticles-multiwall carbon nanotubes-reduced graphene oxide modified glassy carbon electrode was developed. • Simultaneous electrochemical determination of nitrate and nitrite by fabricated sensor was performed. • Modification improved the sensitivity and detection limit of the method. • It is a useful method for determining of nitrate and nitrite in various real samples. - Abstract: In the present research, we aimed to fabricate a novel electrochemical sensor based on Cu metal nanoparticles on the multiwall carbon nanotubes-reduced graphene oxide nanosheets (Cu/MWCNT/RGO) for individual and simultaneous determination of nitrite and nitrate ions. The morphology of the prepared nanocomposite on the surface of glassy carbon electrode (GCE) was characterized using various methods including scanning electron microscopy (SEM), atomic force microscopy (AFM), and electrochemical impedance spectroscopy. Under optimal experimental conditions, the modified GCE showed excellent catalytic activity toward the electro-reduction of nitrite and nitrate ions (pH = 3.0) with a significant increase in cathodic peak currents in comparison with the unmodified GCE. By square wave voltammetry (SWV) the fabricated sensor demonstrated wide dynamic concentration ranges from 0.1 to 75 μM with detection limits (3S_b/m) of 30 nM and 20 nM method for nitrite and nitrate ions, respectively. Furthermore, the applicability of the proposed modified electrode was demonstrated by measuring the concentration of nitrite and nitrate ions in the tap and mineral waters, sausages, salami, and cheese samples.

  3. A sensitive HPLC-MS/MS method for the simultaneous detection of microbial transglutaminase, and bovine and porcine fibrinogen/thrombin in restructured meat.

    Science.gov (United States)

    Jira, Wolfgang; Schwägele, Fredi

    2017-12-15

    A sensitive HPLC-MS/MS method for the simultaneous detection of microbial transglutaminase (TG) from Streptomyces mobaraensis, and bovine and porcine fibrinogen/thrombin in restructured meat was developed using tryptic marker peptides of TG (five markers), and bovine and porcine fibrinogen (six markers each). Meat binding experiments with beef and pork were performed using a technical TG mixture (Activa, Ajinomoto), and bovine and porcine plasmapowder FG (PPFG; Sonac B.V.). The method developed allows the simultaneous detection of the use of these cold-set binders in raw and heated samples. The peak areas of the fibrinogen marker peptides were increased by a factor of about 100, compared to blank values originating from the occurrence of residual blood in meat, using a concentration of 0.6% bovine and porcine PPFG. A differentiation between the use of blood plasma powder and PPFG using the ratios of fibrinogen to serotransferrin peptide peak areas seems to be possible. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Simultaneous determination of ten illegal azo dyes in feed by ultra-high performance liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Piątkowska Marta

    2017-09-01

    Full Text Available Introduction: The paper presents the method of simultaneous determination of 10 illegal azo dyes in feed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry technique. Material and Methods: The dyes were extracted with hexane, evaporated to dryness, and analysed. Separation was achieved in 7 min in a gradient elution using acetonitrile (A and 0.1% formic acid (B as a mobile phase. Results: The validation results showed the repeatability of the method, which was evaluated at three levels (50, 500, and 5,000 μg/kg. All the matrix calibration curves for the working ranges were linear (R2 0.9904 to 1.0, the repeatability was between 2.1% and 24%, and recoveries ranged from 77.9% to 120%. The LOD and LOQ were at 1-2 and 5-10 μg/kg for different dyes, respectively. Furthermore, the method was applied in the homogeneity tests of the in-house prepared feed containing Sudan I at the levels of 0.5, 5, and 50 mg/kg. Conclusions: A sensitive, selective, and fast multiresidue method was successfully developed and validated. Its robustness was confirmed by the analysis of an experimental feed containing Sudan I.

  5. Simultaneous determination of 14N and 15N isotopes in opium by proton induced γ-ray emission technique

    International Nuclear Information System (INIS)

    Pritty Rao; Reddy, G.L.N.; Vikram Kumar, S.; Ramana, J.V.; Raju, V.S.; Sanjiv Kumar

    2012-01-01

    The paper describes the simultaneous determination of 14 N and 15 N isotopes in opium by proton induced γ-ray emission (PIGE) technique. The isotopic ratio of 14 N and 15 N is a useful parameter for assigning provenance of (seized) illicit drugs. The measurement, non-destructive in nature, is performed on pellets made up of opium powders and is based on the prompt detection of 2.313 and 4.4 MeV γ-rays emanating from 14 N(p,p'γ) 14 N and 15 N(p,αγ) 12 C nuclear reactions respectively, induced simultaneously by 3.6-3.8 MeV proton beam. Positive as well as negative deviations from the natural isotopic abundance (99.63:0.37) were observed in the samples. The precision of the measurements is about 4%. The methodology provides an easy and rapid approach to determine the isotopic ratio of 14 N and 15 N and has been used for the first time in the analysis of opium. (author)

  6. Simultaneous Analysis of Monovalent Anions and Cations with a Sub-Microliter Dead-Volume Flow-Through Potentiometric Detector for Ion Chromatography

    Science.gov (United States)

    Dumanli, Rukiye; Attar, Azade; Erci, Vildan; Isildak, Ibrahim

    2016-01-01

    A microliter dead-volume flow-through cell as a potentiometric detector is described in this article for sensitive, selective and simultaneous detection of common monovalent anions and cations in single column ion chromatography for the first time. The detection cell consisted of less selective anion- and cation-selective composite membrane electrodes together with a solid-state composite matrix reference electrode. The simultaneous separation and sensitive detection of sodium (Na+), potassium (K+), ammonium (NH4+), chloride (Cl−) and nitrate (NO3−) in a single run was achieved by using 98% 1.5 mM MgSO4 and 2% acetonitrile eluent with a mixed-bed ion-exchange separation column without suppressor column system. The separation and simultaneous detection of the anions and cations were completed in 6 min at the eluent flow-rate of 0.8 mL/min. Detection limits, at S/N = 3, were ranged from 0.2 to 1.0 µM for the anions and 0.3 to 3.0 µM for the cations, respectively. The developed method was successfully applied to the simultaneous determination of monovalent anions and cations in several environmental and biological samples. PMID:26786906

  7. Simultaneous determination of organophosphorus pesticides and phthalates in baby food samples by ultrasound-vortex-assisted liquid-liquid microextraction and GC-IT/MS.

    Science.gov (United States)

    Notardonato, Ivan; Salimei, Elisabetta; Russo, Mario Vincenzo; Avino, Pasquale

    2018-05-01

    Baby foods are either a soft, liquid paste or an easily chewed food since babies lack developed muscles and teeth to chew effectively. Babies typically move to consuming baby food once nursing or formula is not sufficient for the child's appetite. Some commercial baby foods have been criticized for their contents. This article focuses on the simultaneous determination of organophosphorus pesticides and phthalates by means of a method based on ultrasound-vortex-assisted liquid-liquid microextraction coupled with gas chromatography-ion trap mass spectrometry (GC-IT/MS). The protocol developed allowed the determination of six phthalates [dimethyl phthalate, diethyl phthalate, dibutyl phthalate, isobutyl cyclohexyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate] and 19 organophosphorus pesticides. Freeze-dried product samples (0.1-0.2 g) were dissolved in 10 mL of warm distilled water along with 5 μL of an internal standard (anthracene at 10 mg mL -1 in acetone): the choice of extraction solvent was studied, with the most suitable being n-heptane, which is used for phthalate determination in similar matrices. The solution, held for 5 min in a vortex mixer and for 6 min in a 100-W ultrasonic bath to favor solvent dispersion and consequently analyte extraction, was centrifuged at 4000 rpm for 30 min. Then 1 μL was injected into the GC-IT/MS system (SE-54 capillary column; length 30 m, inner diameter 250 μm, film thickness 0.25 μm). All analytical parameters investigated are discussed in depth. The method was applied to real commercial freeze-dried samples: significant contaminant concentrations were not found. Graphical abstract Simultaneous and sensitive determination of organophosphorus pesticides and phthalates in baby foods by the ultrasound-vortex-assisted liquid-liquid microextraction ֪gas chromatography-ion trap mass spectrometry procedure. 1 methacrifos, 2 pirofos, 3 phorate, 4 seraphos, 5 diazinon, 6 etrimphos, 7 dichlofenthion, 8

  8. Simultaneous determination of water-soluble vitamins in SRM 1849 Infant/Adult Nutritional Formula powder by liquid chromatography-isotope dilution mass spectrometry.

    Science.gov (United States)

    Goldschmidt, Robert J; Wolf, Wayne R

    2010-05-01

    Assessing dietary intake of vitamins from all sources, including foods, dietary supplements, and fortified foods, would be aided considerably by having analytical methodologies that are capable of simultaneous determination of several vitamins. Vitamins naturally present in foods may occur in different chemical forms, with levels ranging over several orders of magnitude. Vitamins in dietary supplements and fortified foods, however, are typically added in a single chemical form, and matrix issues are usually not as complex. These sources should thus be relatively amenable to approaches that aim for simultaneous determination of multiple vitamins. Our recent work has focused on development of liquid chromatography (LC)-UV/fluorescence and LC-tandem mass spectrometry methods for the simultaneous determination of water-soluble vitamins (thiamine, niacin, pyridoxine, pantothenic acid, folic acid, biotin, and riboflavin) in dietary supplement tablets and fortified foods, such as formula powders and breakfast cereals. As part of the validation of our methods and collaboration in characterization of a new NIST SRM 1849 Infant/Adult Nutritional Formula powder, we report data on SRM 1849 using isotope dilution mass spectrometric methods. Use of available NIST Standard Reference Materials(R) as test matrices in our method development and validation gives a benchmark for future application of these methods. We compare three chromatographic approaches and provide data on stability of vitamin standard solutions for LC-based multiple vitamin determinations.

  9. SENSITIVITY ANALYSIS FOR SALTSTONE DISPOSAL UNIT COLUMN DEGRADATION ANALYSES

    Energy Technology Data Exchange (ETDEWEB)

    Flach, G.

    2014-10-28

    PORFLOW related analyses supporting a Sensitivity Analysis for Saltstone Disposal Unit (SDU) column degradation were performed. Previous analyses, Flach and Taylor 2014, used a model in which the SDU columns degraded in a piecewise manner from the top and bottom simultaneously. The current analyses employs a model in which all pieces of the column degrade at the same time. Information was extracted from the analyses which may be useful in determining the distribution of Tc-99 in the various SDUs throughout time and in determining flow balances for the SDUs.

  10. Application of Scion image software to the simultaneous determination of curcuminoids in turmeric (Curcuma longa).

    Science.gov (United States)

    Sotanaphun, Uthai; Phattanawasin, Panadda; Sriphong, Lawan

    2009-01-01

    Curcumin, desmethoxycurcumin and bisdesmethoxycurcumin are bioactive constituents of turmeric (Curcuma longa). Owing to their different potency, quality control of turmeric based on the content of each curcuminoid is more reliable than that based on total curcuminoids. However, to perform such an assay, high-cost instrument is needed. To develop a simple and low-cost method for the simultaneous quantification of three curcuminoids in turmeric using TLC and the public-domain software Scion Image. The image of a TLC chromatogram of turmeric extract was recorded using a digital scanner. The density of the TLC spot of each curcuminoid was analysed by the Scion Image software. The density value was transformed to concentration by comparison with the calibration curve of standard curcuminoids developed on the same TLC plate. The polynomial regression data for all curcuminoids showed good linear relationship with R(2) > 0.99 in the concentration range of 0.375-6 microg/spot. The limits of detection and quantitation were 43-73 and 143-242 ng/spot, respectively. The method gave adequate precision, accuracy and recovery. The contents of each curcuminoid determined using this method were not significantly different from those determined using the TLC densitometric method. TLC image analysis using Scion Image is shown to be a reliable method for the simultaneous analysis of the content of each curcuminoid in turmeric.

  11. Simultaneous square-wave voltammetric determination of aspartame and cyclamate using a boron-doped diamond electrode.

    Science.gov (United States)

    Medeiros, Roberta Antigo; de Carvalho, Adriana Evaristo; Rocha-Filho, Romeu C; Fatibello-Filho, Orlando

    2008-07-30

    A simple and highly selective electrochemical method was developed for the simultaneous determination of aspartame and cyclamate in dietary products at a boron-doped diamond (BDD) electrode. In square-wave voltammetric (SWV) measurements, the BDD electrode was able to separate the oxidation peak potentials of aspartame and cyclamate present in binary mixtures by about 400 mV. The detection limit for aspartame in the presence of 3.0x10(-4) mol L(-1) cyclamate was 4.7x10(-7) mol L(-1), and the detection limit for cyclamate in the presence of 1.0x10(-4) mol L(-1) aspartame was 4.2x10(-6) mol L(-1). When simultaneously changing the concentration of both aspartame and cyclamate in a 0.5 mol L(-1) sulfuric acid solution, the corresponding detection limits were 3.5x10(-7) and 4.5x10(-6) mol L(-1), respectively. The relative standard deviation (R.S.D.) obtained was 1.3% for the 1.0x10(-4) mol L(-1) aspartame solution (n=5) and 1.1% for the 3.0x10(-3) mol L(-1) cyclamate solution. The proposed method was successfully applied in the determination of aspartame in several dietary products with results similar to those obtained using an HPLC method at 95% confidence level.

  12. A new electrochemical sensor for the simultaneous determination of acetaminophen and codeine based on porous silicon/palladium nanostructure.

    Science.gov (United States)

    Ensafi, Ali A; Ahmadi, Najmeh; Rezaei, Behzad; Abarghoui, Mehdi Mokhtari

    2015-03-01

    A porous silicon/palladium nanostructure was prepared and used as a new electrode material for the simultaneous determination of acetaminophen (ACT) and codeine (COD). Palladium nanoparticles were assembled on porous silicon (PSi) microparticles by a simple redox reaction between the Pd precursor and PSi in an aqueous solution of hydrofluoric acid. This novel nanostructure was characterized by different spectroscopic and electrochemical techniques including scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, fourier transform infrared spectroscopy and cyclic voltammetry. The high electrochemical activity, fast electron transfer rate, high surface area and good antifouling properties of this nanostructure enhanced the oxidation peak currents and reduced the peak potentials of ACT and COD at the surface of the proposed sensor. Simultaneous determination of ACT and COD was explored using differential pulse voltammetry. A linear range of 1.0-700.0 µmol L(-1) was achieved for ACT and COD with detection limits of 0.4 and 0.3 µmol L(-1), respectively. Finally, the proposed method was used for the determination of ACT and COD in blood serum, urine and pharmaceutical compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Simultaneous HPTLC Determination of Rabeprazole and Itopride Hydrochloride From Their Combined Dosage Form.

    Science.gov (United States)

    Suganthi, A; John, Sofiya; Ravi, T K

    2008-01-01

    A simple, precise, sensitive, rapid and reproducible HPTLC method for the simultaneous estimation of the rabeprazole and itopride hydrochloride in tablets was developed and validated. This method involves separation of the components by TLC on precoated silica gel G60F254 plate with solvent system of n-butanol, toluene and ammonia (8.5:0.5:1 v/v/v) and detection was carried out densitometrically using a UV detector at 288 nm in absorbance mode. This system was found to give compact spots for rabeprazole (Rf value of 0.23 0.02) and for itopride hydrochloride (Rf value of 0.75+/-0.02). Linearity was found to be in the range of 40-200 ng/spot and 300-1500 ng/spot for rabeprazole and itopride hydrochloride. The limit of detection and limit of quantification for rabeprazole were 10 and 20 ng/spot and for itopride hydrochloride were 50 and 100 ng/spot, respectively. The method was found to be beneficial for the routine analysis of combined dosage form.

  14. Simultaneous determination of seven anticoagulant rodenticides in agricultural products by gel permeation chromatography and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saito-Shida, Shizuka; Nemoto, Satoru; Matsuda, Rieko; Akiyama, Hiroshi

    2016-11-01

    A sensitive and reliable method for the simultaneous determination of hydroxycoumarin-type (brodifacoum, bromadiolone, coumatetralyl, and warfarin) and indandione-type (chlorophacinone, diphacinone, and pindone) rodenticides in agricultural products by gel permeation chromatography (GPC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The procedure involved extraction of the rodenticides from samples with acetone, followed by liquid-liquid partitioning with hexane/ethyl acetate (1:1, v/v) and 10% sodium chloride aqueous solution, then cleanup using GPC, and finally, analysis using LC-MS/MS. High recoveries from the GPC column were obtained for all rodenticides tested using a mobile phase of acetone/cyclohexane/triethylamine (400:1600:1, v/v/v). An ODS column, which contains low levels of metal impurities, gave satisfactory peak shapes for both hydroxycoumarin- and indandione-type rodenticides in the LC-MS/MS separation. The average recoveries of rodenticides from eight agricultural foods (apple, eggplant, cabbage, orange, potato, tomato, brown rice, and soybean) fortified at 0.0005-0.001 mg/kg ranged from 76 to 116%, except for bromadiolone in orange (53%) and diphacinone in soybean (54%), and the relative standard deviations ranged from 1 to 16%. The proposed method effectively removed interfering components, such as pigments and lipids, and showed high selectivity. In addition, the matrix effects were negligible for most of the rodenticide/food combinations. The results suggest that the proposed method is reliable and suitable for determining hydroxycoumarin- and indandione-type rodenticides in agricultural products.

  15. An isocratic HPLC method for the simultaneous determination of cholesterol, cardiolipin, and DOPC in lyophilized lipids and liposomal formulations.

    Science.gov (United States)

    Simonzadeh, Ninus

    2009-04-01

    Phospholipids, such as 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC), and 1,1',2,2'-tetramyristoyl cardiolipin, along with cholesterol, form liposomes in aqueous media and have been investigated at NeoPharm (Lake Bluff, IL) as drug-delivery systems. To accurately assess the effectiveness of various formulations involving the use of aforementioned phospholipids and cholesterol, their quantitative determination is essential. An isocratic high-performance liquid chromatographic method for the simultaneous determination of cholesterol, cardiolipin, and DOPC in various pharmaceutical formulations containing the active drug substance has consequently been developed and is presented here. The current method utilizes an ASTEC-diol analytical column and is shown to be stability-indicating and free from interference from any of the formulation excipients, such as sucrose, sodium chloride, and sodium lactate. The analytes are detected using an evaporative light scattering detector (Alltech or Polymer Laboratories). The quantitation of each lipid component is performed using non-linear regression analysis. The retention characteristics of the analytes are examined as a function of eluent composition (e.g., pH, salt content, organic to aqueous phase ratio) and column temperature. The method was validated and was found to be sensitive, specific, rugged, and cost-effective. The current method provides enhanced chromatographic separation for lipid components as well as degradation products as compared to similar methods reported in the literature. It is also inherently simpler than other similar methods reported in the literature that typically use complex gradient elution.

  16. A simple and sensitive method for determination of Norfloxacin in pharmaceutical preparations

    Directory of Open Access Journals (Sweden)

    Zhuo Ye

    2015-06-01

    Full Text Available In this approach, a new voltammetric method for determination of norfloxacin was proposed with high sensitivity and wider detection linear range. The used voltammetric sensor was fabricated simply by coating a layer of graphene oxide (GO and Nafion composited film on glassy carbon electrode. The advantage of proposed method was sensitive electrochemical response for norfloxacin, which was attributed to the excellent electrical conductivity of GO and the accumulating function of Nafion under optimum experimental conditions, the present method revealed a good linear response for determination of norfloxacin in the range of 1×10-8mol/L-7×10-6 mol/L with a detection limit of 5×10-9 mol/L. The proposed method was successfully applied in the determination of norfloxacin in capsules with satisfactory results.

  17. Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers

    International Nuclear Information System (INIS)

    Kovtun, J.L.; Miroshnikova, N.N.; Saveliev, I.B.; Sidorov, A.V.; Srapeniants, R.A.; Tsagolov, K.S.

    1981-01-01

    According to the invention, the radioactivation method for simultaneous determination of the nitrogen, phosphorus and potassium content in plants and fertilizers consists in exposing samples to be analyzed and standard samples to neutron irradiation and recording the spectra of the gamma radiation induced in said samples, whereupon the samples are laid aside for a period of time determined by the half-life of the interfering isotope. This is followed by again recording the spectra of the samples being analyzed and of the standard samples and superposing the first and second spectra of the samples being analyzed and of the standard samples. These spectra are then shifted relative to each other along the energy axis, and the contents of the elements being analyzed are determined by thus comparing the spectra of the samples being analyzed and of the standard samples

  18. Three-dimensional activated graphene network-sulfonate-terminated polymer nanocomposite as a new electrode material for the sensitive determination of dopamine and heavy metal ions.

    Science.gov (United States)

    Yuan, Xiaoyan; Zhang, Yijia; Yang, Lu; Deng, Wenfang; Tan, Yueming; Ma, Ming; Xie, Qingji

    2015-03-07

    We report here that three-dimensional activated graphene networks (3DAGNs) are a better matrix to prepare graphene-polymer nanocomposites for sensitive electroanalysis than two-dimensional graphene nanosheets (2DGNs). 3DAGNs were synthesized in advance by the direct carbonization and simultaneous chemical activation of a cobalt ion-impregnated D113-type ion exchange resin, which showed an interconnected network structure and a large specific surface area. Then, the 3DAGN-sulfonate-terminated polymer (STP) nanocomposite was prepared via the in situ chemical co-polymerization of m-aminobenzene sulfonic acid and aniline in the presence of 3DAGNs. The 3DAGN-STP nanocomposite can adsorb dopamine (DA) and heavy metal ions, which was confirmed by quartz crystal microbalance studies. The 3DAGN-STP modified glassy carbon electrode (GCE) was used for the electrochemical detection of DA in the presence of ascorbic acid and uric acid, with a linear response range of 0.1-32 μM and a limit of detection of 10 nM. In addition, differential pulse voltammetry was used for the simultaneous determination of Cd(2+) and Pb(2+) at the 3DAGN-STP/GCE further modified with a bismuth film, exhibiting linear response ranges of 1-70 μg L(-1) for Cd(2+) and 1-80 μg L(-1) for Pb(2+) with limits of detection of 0.1 μg L(-1) for Cd(2+) and 0.2 μg L(-1) for Pb(2+). Because the 3DAGN-STP can integrate the advantages of 3DAGNs with STPs, the 3DAGN-STP/GCE was more sensitive than the bare GCE, 3DAGN/GCE, and 2DGN-STP/GCE for the determination of DA and heavy metal ions.

  19. [Simultaneous determination of 15 polycyclic aromatic hydrocarbons in cigarette filter by gas chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Xiaotao; Zhang, Li; Ruan, Yibin; Wang, Weiwei; Ji, Houwei; Wan, Qiang; Lin, Fucheng; Liu, Jian

    2017-10-08

    A method for the simultaneous determination of 15 polycyclic aromatic hydrocarbons in cigarette filter was developed by isotope internal standard combined with gas chromatography-tandem mass spectrometry. The cigarette filters were extracted with dichloromethane, and the extract was filtered with 0.22 μm organic phase membrane. The samples were isolated by DB-5MS column (30 m×0.25 mm, 0.25 μm) and detected using multiple reaction monitoring mode of electron impact source under positive ion mode. The linearities of the 15 polycyclic aromatic hydrocarbons (acenapthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, ben[ a ]anthracene, chrysene, benzo[ b ]fluoranthene, benzo[ k ]fluoranthene, benzo[ a ]pyrene, dibenzo[ a,h ]anthracene, benzo[ g,h,i ]perylene and indeno[1,2,3- c,d ]pyrene) were good, and the correlation coefficients ( R 2 ) ranged from 0.9914 to 0.9999. The average recoveries of the 15 polycyclic aromatic hydrocarbons were 81.6%-109.6% at low, middle and high spiked levels, and the relative standard deviations were less than 16%, except that the relative standard deviation of fluorene at the low spiked level was 19.2%. The limits of detection of the 15 polycyclic aromatic hydrocarbons were 0.02 to 0.24 ng/filter, and the limits of quantification were 0.04 to 0.80 ng/filter. The method is simple, rapid, accurate, sensitive and reproducible. It is suitable for the quantitative analysis of the 15 polycyclic aromatic hydrocarbons in cigarette filters.

  20. Development of a system for simultaneous - sequential determinations of major and minor actinides (Th, Np, U, Pu, Am, Cm) by on-line extraction chromatography - ion concentration - inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Trivellone, E.; Mariani, M.; Carlos-Marquez, R.; Aldave de las Heras, L.; Betti, M.; )

    2009-01-01

    Full text: Because of the great complexity and time consuming of traditional methods for actinides determination, a procedure for their simultaneous and sequential separation and quantification was developed. A complete circuit constituted by three analytical chromatographic columns packed with TEVA, UTEVA and TRU resins (Eichrom Inc) for retention of tetra-, hexa- and tri-valent actinides and three cation concentrator columns TCC-II (from Dionex Corporation) connected by six (4-way and 6-way) valves is coupled on-line to an ICPMS detector. The use of TCC-II columns just prior of the ICPMS determination allows to improve sensitivity and detection limits down to the ng/l level. The use of a coupled HPLC to an ICPMS system enables the complete analysis of all the six actinides in almost 2 hours. (author)

  1. Determinants of long-term outcome in patients undergoing simultaneous resection of synchronous colorectal liver metastases.

    Directory of Open Access Journals (Sweden)

    Qi Lin

    Full Text Available BACKGROUND: It remains unclear which patients can benefit from simultaneous resection of synchronous colorectal liver metastases (SCRLMs. This study aimed to examine the prognostic value of patient- and tumor-related factors in predicting long-term outcomes of patients undergoing simultaneous resection of SCRLMs and to help patients select a suitable therapeutic regimen and proper surveillance. METHODS: Clinicopathological and outcome data of 154 consecutive SCRLM patients who underwent simultaneous resection between July 2003 and July 2013 were collected from our prospectively established SCRLM data and analyzed with univariate and multivariate methods, and the prognostic index (PI was formulated based on the regression coefficients (β of the Cox model. The patients were classified into high- and low-risk groups according to the PI value; the cut-off point was the third quartile. RESULTS: The 5-year overall survival rate was 46%, and the 5-year disease-free survival rate was 35%. Five factors were found to be independent predictors of poor overall survival (OS by multivariate analysis: positive lymph node status, vascular invasion, BRAF mutation, the distribution of bilobar liver metastases (LMs and non-R0 resection of LMs. Compared to low PI (≤5.978, high PI (>5.978 was highly predictive of shorter OS. Three factors were found to be independent predictors of poor disease-free survival (DFS by multivariate analysis: tumor deposits, BRAF mutation and bilobar LM distribution. We also determined the PI for DFS. Compared to low PI (≤2.945, high PI (>2.945 was highly predictive of shorter DFS. CONCLUSIONS: Simultaneous resection of SCRLM may lead to various long-term outcomes. Patients with low PI have longer OS and DFS, while those with high PI have shorter OS and DFS. Thus, patients with high PI may receive more aggressive treatment and intensive surveillance, This model needs further validation.

  2. The simultaneous boost technique

    International Nuclear Information System (INIS)

    Lebesque, J.V.; Keus, R.B.

    1991-01-01

    Simultaneous boost technique in radiotherapy consists of delivering the boost treatment (additional doses to reduced volumes) simultaneously with the basic (large-field) treatment for all treatment sessions. Both the dose per fraction delivered by basic-treatment fields and by boost-treatment fields have to be reduced to end up with the same total dose in boost volume as in the original schedule, where basic treatment preceded boost treatment. These dose reductions and corresponding weighting factors have been calculated using the linear-quadratic (LQ) model and the concept of Normalized Total Dose (NTD). Relative NTD distributions were computed to evaluate the dose distributions resulting for the simultaneous boost technique with respect to acute and late normal tissue damage and tumor control. For the example of treatment of prostate cancer the weighting factors were calculated on basis of NTD for late normal tissue damage. For treatment of oropharyngeal cancer NTD for acute and normal tissue damage was used to determine the weighting factors. In this last example a theoretical sparing of late normal tissue damage can be demonstrated. Another advantage of simultaneous boost technique is that megavoltage images of the large basic-treatment fields facilitates the determination of the position of the patient with respect to the small boost-treatment fields. (author). 42 refs., 8 figs

  3. Validation Study on a Rapid Method for Simultaneous Determination of Pesticide Residues in Vegetables and Fruits by LC-MS/MS.

    Science.gov (United States)

    Sato, Tamaki; Miyamoto, Iori; Uemura, Masako; Nakatani, Tadashi; Kakutani, Naoya; Yamano, Tetsuo

    2016-01-01

    A validation study was carried out on a rapid method for the simultaneous determination of pesticide residues in vegetables and fruits by LC-MS/MS. Preparation of the test solution was performed by a solid-phase extraction technique with QuEChERS (STQ method). Pesticide residues were extracted with acetonitrile using a homogenizer, followed by salting-out and dehydration at the same time. The acetonitrile layer was purified with C18 and PSA mini-columns. The method was assessed for 130 pesticide residues in 14 kinds of vegetables and fruits at the concentration level of 0.01 μg/g according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. As a result 75 to 120 pesticide residues were determined satisfactorily in the tested samples. Thus, this method could be useful for a rapid and simultaneous determination of multi-class pesticide residues in various vegetables and fruits.

  4. Physical determinants of radiation sensitivity in bacterial spores

    International Nuclear Information System (INIS)

    Powers, E.L.

    1982-01-01

    Several factors modifying radiation sensitivity in dry bacterial spores are described and discussed. Vacuum inducing the loss of critical structural water, very low dose rates of radiation from which the cell may recover, radiations of high linear energy transfer, and the action of temperature over long periods of time on previously irradiated cells are recognized from extensive laboratory work as important in determining survival of spores exposed to low radiation doses at low temperatures for long periods of time. Some extensions of laboratory work are proposed

  5. Simultaneous Determination of Acetaminophen and Synthetic Color(s) by Derivative Spectroscopy in Syrup Formulations and Validation by HPLC: Exposure Risk of Colors to Children.

    Science.gov (United States)

    Rastogi, Shanya Das; Dixit, Sumita; Tripathi, Anurag; Das, Mukul

    2015-06-01

    Color additives are used in pediatric syrup formulations as an excipient; though not pre-requisite, but pediatric syrup formulations are normally colored. An attempt has been made to measure simultaneously the single drug, acetaminophen (AT), along with the colors, carmoisine (CA), erythrosine (ET), and sunset yellow FCF (SSY) added in it by three derivative spectroscopy methods namely, 1st order, ratio, and differential derivative methods. Moreover, evaluation has been made for the exposure assessment of the colors added as excipient because some colors have been reported to cause allergic reactions and hypersensitivity in children. The present methods provide simple, accurate, and reproducible quantitative determination of the drug, AT, along with the color in synthetic mixtures and commercial drug formulations without any interference. The limit of detection varied from 0.0001-0.31 μg/ml while limit of quantification ranged from 0.002-1.04 μg/ml in all the three methods. The calibration curve of all the three derivative methods exhibited good linear relationship with excellent regression coefficients (0.9986-1.000). Both intra-day and inter-day precisions showed %RSD value less than 2% while the percentage recovery was found between 96.8-103.8%. The sensitivity of the proposed methods is almost comparable to HPLC and thus, can be used for determination of drug AT, and color simultaneously in pharmaceutical formulation on routine basis. The present methods also showed that colors like SSY and ET are saturating more than 50% of acceptable daily intake (ADI) value which is alarming and needs to be considered for modification by regulatory authorities to safeguard the health of children.

  6. Simultaneous Determination of Hydroquinone, Catechol and Resorcinol at Graphene Doped Carbon Ionic Liquid Electrode

    Directory of Open Access Journals (Sweden)

    Li Ma

    2012-01-01

    Full Text Available A new composite electrode has been prepared with doping graphene into the paste consisting graphite and ionic liquid, n-octyl-pyridinum hexafluorophosphate (OPFP. This electrode shows an excellent electrochemical activity for the redox of hydroquinone (HQ, catechol (CC, and resorcinol (RS. In comparison with bare paste electrode, the redox peaks of three isomers of dihydroxybenzene can be obviously, simultaneously observed at graphene doping paste electrode. Under the optimized condition, the simultaneous determination of HQ, CC, and RS in their ternary mixture can be carried out with a differential pulse voltammetric technique. The peak currents are linear to the concentration of HQ, CC, and RS in the range form 1×10−5 to 4×10−4, 1×10−5 to 3×10−4, and 1×10−6 to 1.7×10−4 mol L−1, respectively. The limits of detection are 1.8×10−6 mol L−1 for HQ, 7.4×10−7 mol L−1 for CC, and 3.6×10−7 M for RS, respectively.

  7. Rapid and simultaneous determination of polychlorinated biphenyls and their main metabolites (hydroxylated and methyl sulfonyl) by gas chromatography coupled to mass spectrometry: Comparison of different ionisation modes

    International Nuclear Information System (INIS)

    Castro-Puyana, M.; Herrero, L.; González, M.J.; Gómara, B.

    2013-01-01

    Graphical abstract: -- Highlights: •Simultaneous determination of PCB, OH-PCBs and MeSO 2 -PCBs in a single GC–MS run. •Two different ionisation modes (EI and ECNI) are studied and compared. •The analytical characterisation of both methods is satisfactory. •Better LODs are achieved using ECNI-MS as ionisation mode. •The developed methodology is successfully applied to fish liver oil. -- Abstract: Instrumental methods based on gas chromatography coupled to mass spectrometry (GC–MS) have been developed and compared using two different MS ionisation modes, electron impact (EI) and electron capture negative ionisation (ECNI), for the fast, quantitative and simultaneous determination of polychlorinated biphenyls (PCBs) and their main metabolites (hydroxylated PCBs, OH-PCBs, and methyl sulfone PCBs, MeSO 2 -PCBs). Parameters affecting chromatographic separation and MS detection were evaluated in order to achieve the highest selectivity and sensitivity for both operation modes. The analytical characteristics of the developed methods were studied and compared in terms of linear range, limits of detection (LODs), limits of quantification (LOQs), and instrumental precision (repeatability and intermediate precision). Both ionisation methods showed similar precision, being relative standard deviations (RSD, %) lower than 9% and 14% for repeatability and intermediate precision, respectively. However, better LODs (from 0.01 to 0.14 pg injected for the three families of congeners studied) were achieved using ECNI-MS as ionisation mode. The suitability of the developed method was demonstrated through their application to fish liver oil samples

  8. Development of the kits for RIA simultaneous determination of polypeptide hormones

    International Nuclear Information System (INIS)

    Szybinski, Z.

    1982-12-01

    A simple and universal modification of chloramine T technique has been developed for the radioactive iodination of several polypeptide hormones such as insulin, human growth hormone (HGH), human TSH, synthetic human gastrin and beta-endorphine. The prepared products proved to have good immunoreactivity suitable for RIA purposes. The technique is inexpensive and quick. A new procedure has also been worked out utilizing horse myeloperoxidase in solid state as catalyser. The hormones iodinated with this technique show better parameters (e.g. longer stability, better binding to antibody, more favourable adsorption on dextran-coated charcoal); however the specific activities achieved were lower. The possibilities of simultaneous measurement of insulin and HGH have been studied. In this connection, a comparatively simple method for the determination of the endogenous anti-insulin antibodies was developed and used for the control of patients with diabetes and for the checking of new insulin preparations. However, the technique requires relatively sophisticated equipment and computerized calculations

  9. Simultaneous determination of five active compounds in chimonanthus nitens by double-development HPTLC and scanning densitometry

    Directory of Open Access Journals (Sweden)

    Zhou Bin

    2012-05-01

    Full Text Available Abstract Background Chimonanthus nitens (family Calycanthaceae, Shanlamei in Chinese, is an unique species in China. The extract of dried leaves of Chimonanthus nitens has anti-inflammatory, antipyretic and antitussive effects. Terpenes, coumarins, and flavonoids are usually regarded as the main active components. Therefore, simultaneous determination of these compounds is very important to control the quality of Chimonanthus nitens. Results A double-development TLC method was developed for simultaneous analysis of five compounds in Chimonanthus nitens. The chromatography was performed on silica gel 60 plate with chloroform-methanol (9∶1, v/v and petroleum ether-ethyl acetate (10∶1, v/v as mobile phase for twice development. Their characteristic TLC profiles were observed under UV light at 365 nm and the bands were then revealed by reaction with 1% vanillin-H2SO4 solution. Quantification of three monoterpenes was achieved by densitometry at 545 nm (β-caryophyllene or 606 nm (cineole and linalool. Two coumarins (scopoletin and scoparone were determined by densitometry at 340 nm with filter wavelength of 370 nm. The investigated compounds had good linearity (R2 >0.99 within test ranges. Conclusions The developed double-development TLC method is helpful to control the quality of Chimonanthus nitens, which is simple and accurate.

  10. Screen-printed electrodes modified with carbon nanotubes or graphene for simultaneous determination of melatonin and serotonin

    International Nuclear Information System (INIS)

    Gomez, Federico José Vicente; Martín, Aída; Escarpa, Alberto; Silva, María Fernanda

    2015-01-01

    Single-walled carbon nanotubes (SWCNT), multi-walled carbon nanotubes (MWCNT) and graphene have been tested as carbon allotropes for the modification of carbon screen-printed electrodes (CSPEs) to simultaneously determine melatonin (MT) and serotonin (5-HT). Two groups of CSPEs, both 4 mm in diameter, were explored: The first includes commercial SWCNT, MWCNT and graphene, the second includes SWCNT, MWCNT, graphene oxide nanoribbons and reduced nanoribbons that were drop casted on the electrodes. The carbon nanomaterials enhanced the electroactive area in the following order: CSPE simultaneous determination of 5-HT and MT at the working potentials of +50 mV and +390 mV (vs. Ag), respectively. The use of carbon nanomaterials, in particular of graphene oxide nanoribbons on CSPEs, represents an excellent and disposable tool for sensing the two target molecules in even small sample volumes. Figures of merit for MT and 5-HT include (a) detection limit of 1.1 and 0.4 μM for MT and 5-HT, respectively; (b) an inter-electrode reproducibility with RSD ≤ 8 %; (c) 120 s response time, and (d) recoveries (in case of spiked samples) ranging from 94 to 103 % (with an RSD < 1 %). (author)

  11. Separation and Simultaneous Determination of 14 Fungicides with the Combination of Multi-Analyte Methods and HPLC Detection

    Energy Technology Data Exchange (ETDEWEB)

    Canping, Pan [Department of Applied Chemistry, China Agricultural University, Beijing (China)

    2009-07-15

    The separation and simultaneous HPLC-MS determination for a series of fungicide products is reported. Multi-analyte methods were applied on a Chromolith RP-18e monolithic column having low resistance and enabling high flow rates and short analysis time at very good separation power. Details and analytical conditions are described with chromatograms illustrating the results and work done. (author)

  12. Simultaneity, relativity and conventionality

    Science.gov (United States)

    Janis, Allen I.

    2008-01-01

    The view of simultaneity presented by Max Jammer is almost breathtaking, encompassing, as the book's subtitle suggests, the period from antiquity to the 21st century. Many interesting things are to be found along the way. For example, what Jammer (p. 49) says "may well be regarded as probably the earliest recorded example of an operational definition of distant simultaneity" is due to St. Augustine (in his Confessions, written in 397 A.D.; for a modern translation, see Augustine, 2006). He was arguing against astrology by presenting the story of two women, one rich and one poor, who gave birth simultaneously. Although the two children thus had precisely the same horoscopes, their lives followed quite different courses. And how was it determined that the births were simultaneous? A messenger went from each birth site to the other, leaving the instant the child was born (and, presumably, traveling with equal speeds). Since the messengers met at the midpoint between the locations of the two births, the births must have been simultaneous. This is, of course, quite analogous to Albert Einstein's definition of simultaneity (given more than 1500 years later), which will be discussed in Section 2.1.

  13. Simultaneous Determination of Cobalt (II and Nickel (II By First Order Derivative Spectrophotometry in Micellar Media

    Directory of Open Access Journals (Sweden)

    Rajni Rohilla

    2012-01-01

    Full Text Available A first-derivative spectrophotometry method for the simultaneous determination of Co (II and Ni (II with Alizarin Red S in presence of Triton X-100 is described. Measurements were made at the zero-crossing wavelengths at 549.0 nm for Co (II and 546.0 nm for Ni (II. The linearity is obtained in the range of 0.291- 4.676 μg/ml of Ni (II and 0.293- 4.124 μg/ml of Co (II in the presence of each other by using first derivative spectrophotometric method. The possible interfering effects of various ions were studied. The validity of the method was examined by using synthetic mixtures of Co (II and Ni (II. The developed derivative procedure, using the zero crossing technique, has been successfully applied for the simultaneous analysis of Co (II and Ni (II in spiked water samples.

  14. Simultaneous determination of amino acids and neurotransmitters in plasma samples from schizophrenic patients by hydrophilic interaction liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Domingues, Diego Soares; Crevelin, Eduardo José; de Moraes, Luiz Alberto Beraldo; Cecilio Hallak, Jaime Eduardo; de Souza Crippa, José Alexandre; Costa Queiroz, Maria Eugênia

    2015-03-01

    A sensitive, reproducible, and rapid method was developed for the simultaneous determination of underivatized amino acids (aspartate, serine, glycine, alanine, methionine, leucine, tyrosine, and tryptophan) and neurotransmitters (glutamate and γ-aminobutyric acid) in plasma samples using hydrophilic interaction liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The plasma concentrations of amino acids and neurotransmitters obtained from 35 schizophrenic patients in treatment with clozapine (27 patients) and olanzapine (eight patients) were compared with those obtained from 38 healthy volunteers to monitor the effectiveness of treatment. The chromatographic conditions separated ten target compounds within 3 min. This method presented linear ranges that varied from (lower limit of quantification: 9.7-13.3 nmol/mL) to (upper limit of quantification: 19.4-800 nmol/mL), intra- and interassay precision with coefficients of variation lower than 10%, and relative standard error values of the accuracy ranged from -2.1 to 9.9%. The proposed method appropriately determines amino acids and neurotransmitters in plasma from schizophrenic patients. Compared with the control group (healthy volunteers), the plasma levels of methionine in schizophrenic patients treated with olanzapine are statistically significantly higher. Moreover, schizophrenic patients treated with clozapine tend to have increased plasma levels of glutamate. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Simultaneous high-performance liquid chromatographic determination of nitrate, nitrite, and organic pesticides in soil solution using a multidimensional column with ultraviolet detection

    International Nuclear Information System (INIS)

    Nkedi-Kizza, P.; Owusu-Yaw, J.

    1992-01-01

    In many fertilizer trials, the amount of nitrate-nitrogen in soil solution must be quantified frequently because nitrate is easily leached. Because pesticides are generally applied to cropland with fertilizers, quantitative information is needed on the concentration of these chemicals still available in the soil. Information on nitrite, nitrate and pesticide concentrations in food, water and environmental samples is essential because of their toxicity and potential for groundwater and surface water contamination. Most of the methods currently used for nitrate determination also account for nitrite, because nitrite and some organics act as interferences. Some of the existing analytical methods require sample reduction or derivatization, complex solvent mixtures or large sample volumes which make analysis times long. A High-Performance Liquid Chromatography (HPLC) method has been developed for the simultaneous determination of nitrate, nitrite and organic pesticides in soil solution samples and extracts using a multidimensional separator column with ultraviolet detection at 220 nm. The method is rapid and requires small sample volumes (20 μL). It is a sensitive method which is suitable for routine analyses of up to 100 samples per day. A comparison of this method with standard ion chromatography with conductivity detection showed very good agreement between the two methods for the analysis of NO3- and NO2-

  16. Simultaneous Determination of Food-Related Biogenic Amines and Precursor Amino Acids Using in Situ Derivatization Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction by Ultra-High-Performance Liquid Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    He, Yongrui; Zhao, Xian-En; Wang, Renjun; Wei, Na; Sun, Jing; Dang, Jun; Chen, Guang; Liu, Zhiqiang; Zhu, Shuyun; You, Jinmao

    2016-11-02

    A simple, rapid, sensitive, selective, and environmentally friendly method, based on in situ derivatization ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) coupled with ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) using multiple reaction monitoring (MRM) mode has been developed for the simultaneous determination of food-related biogenic amines and amino acids. A new mass-spectrometry-sensitive derivatization reagent 4'-carbonyl chloride rosamine (CCR) was designed, synthesized, and first reported. Parameters and conditions of in situ DUADLLME and UHPLC-MS/MS were optimized in detail. Under the optimized conditions, the in situ DUADLLME was completed speedily (within 1 min) with high derivatization efficiencies (≥98.5%). With the cleanup and concentration of microextraction step, good analytical performance was obtained for the analytes. The results showed that this method was accurate and practical for quantification of biogenic amines and amino acids in common food samples (red wine, beer, wine, cheese, sausage, and fish).

  17. Some problems connected with boron determination by atomic absorption spectroscopy and the sensitivity improvement

    Directory of Open Access Journals (Sweden)

    JELENA J. SAVOVIC

    2001-08-01

    Full Text Available Two atomizers were compared: an N2O–C2H2 flame and a stabilized U-shaped DC arc with aerosol supply. Both the high plasma temperature and the reducing atmosphere obtained by acetylene addition to the argon stream substantially increase the sensitivity of boron determination by atomic absorption spectroscopy (AAS when the arc atomizer is used. The results were compared with those for silicon as a control element. The experimental characteristic concentrations for both elements were compared with the computed values. The experimentally obtained characteristic concentration for boron when using the arc atomizer was in better agreement with the calculated value. It was estimated that the influence of stable monoxide formation on the sensitivity for both elements was about the same, but reduction of analyte and formation of non-volatile carbide particles was more important for boron, which is the main reason for the low sensitivity of boron determination using a flame atomizer. The use of an arc atomizer suppresses this interference and significantly improves the sensitivity of the determination.

  18. Multiplex Real-Time qPCR Assay for Simultaneous and Sensitive Detection of Phytoplasmas in Sesame Plants and Insect Vectors.

    Science.gov (United States)

    Ikten, Cengiz; Ustun, Rustem; Catal, Mursel; Yol, Engin; Uzun, Bulent

    2016-01-01

    Phyllody, a destructive and economically important disease worldwide caused by phytoplasma infections, is characterized by the abnormal development of floral structures into stunted leafy parts and contributes to serious losses in crop plants, including sesame (Sesamum indicum L.). Accurate identification, differentiation, and quantification of phyllody-causing phytoplasmas are essential for effective management of this plant disease and for selection of resistant sesame varieties. In this study, a diagnostic multiplex qPCR assay was developed using TaqMan® chemistry based on detection of the 16S ribosomal RNA gene of phytoplasmas and the 18S ribosomal gene of sesame. Phytoplasma and sesame specific primers and probes labeled with different fluorescent dyes were used for simultaneous amplification of 16SrII and 16SrIX phytoplasmas in a single tube. The multiplex real-time qPCR assay allowed accurate detection, differentiation, and quantification of 16SrII and 16SrIX groups in 109 sesame plant and 92 insect vector samples tested. The assay was found to have a detection sensitivity of 1.8 x 102 and 1.6 x 102 DNA copies for absolute quantification of 16SrII and 16SrIX group phytoplasmas, respectively. Relative quantification was effective and reliable for determination of phyllody phytoplasma DNA amounts normalized to sesame DNA in infected plant tissues. The development of this qPCR assay provides a method for the rapid measurement of infection loads to identify resistance levels of sesame genotypes against phyllody phytoplasma disease.

  19. Simultaneous determination of organophosphorus pesticides in fruits and vegetables using atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry.

    Science.gov (United States)

    Cheng, Zhipeng; Dong, Fengshou; Xu, Jun; Liu, Xingang; Wu, Xiaohu; Chen, Zenglong; Pan, Xinglu; Gan, Jay; Zheng, Yongquan

    2017-09-15

    This paper describes the application of atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for the simultaneous determination of organophosphorus pesticides in apple, pear, tomato, cucumber and cabbage. Soft ionization with atmospheric pressure ionization source was compared with traditional electron impact ionization (EI). The sensitivity of GC coupled to atmospheric pressure ionization (APGC) for all the analytes was enhanced by 1.0-8.2 times. The ionization modes with atmospheric pressure ionization source was studied by comparing the charge-transfer and proton-transfer conditions. The optimized QuEChERs method was used to pretreat the samples. The calibration curves were found linear from 10 to 1000μg/L, obtaining correlation coefficients higher than 0.9845. Satisfactory mean recovery values, in the range of 70.0-115.9%, and satisfactory precision, with all RSD r <19.7% and all RSD R values <19.5% at the three fortified concentration levels for all the fifteen OPPs. The results demonstrate the potential of APGC-QTOF-MS for routine quantitative analysis of organophosphorus pesticide in fruits and vegetables. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Multiplexed Simultaneous High Sensitivity Sensors with High-Order Mode Based on the Integration of Photonic Crystal 1 × 3 Beam Splitter and Three Different Single-Slot PCNCs.

    Science.gov (United States)

    Zhou, Jian; Huang, Lijun; Fu, Zhongyuan; Sun, Fujun; Tian, Huiping

    2016-07-07

    We simulated an efficient method for the sensor array of high-sensitivity single-slot photonic crystal nanobeam cavities (PCNCs) on a silicon platform. With the combination of a well-designed photonic crystal waveguide (PhCW) filter and an elaborate single-slot PCNC, a specific high-order resonant mode was filtered for sensing. A 1 × 3 beam splitter carefully established was implemented to split channels and integrate three sensors to realize microarrays. By applying the three-dimensional finite-difference-time-domain (3D-FDTD) method, the sensitivities calculated were S₁ = 492 nm/RIU, S₂ = 244 nm/RIU, and S₃ = 552 nm/RIU, respectively. To the best of our knowledge, this is the first multiplexing design in which each sensor cite features such a high sensitivity simultaneously.

  1. Development of Reverse-Phase HPLC Method for Simultaneous ...

    African Journals Online (AJOL)

    Erah

    Purpose: To develop a simple, sensitive and rapid reverse phase HPLC method for the simultaneous analysis of metoprolol succinate and hydrochlorothiazide in a solid dosage form. Methods: The .... Extraction was carried out three times with.

  2. Effects of simultaneous exposure to stress and nicotine on nicotine-induced locomotor activation in adolescent and adult rats

    Directory of Open Access Journals (Sweden)

    A. Zago

    2012-01-01

    Full Text Available Preclinical studies have shown that repeated stress experiences can result in an increase in the locomotor response to the subsequent administration of drugs of abuse, a phenomenon that has been termed behavioral cross-sensitization. Behavioral sensitization reflects neuroadaptive processes associated with drug addiction and drug-induced psychosis. Although cross-sensitization between stress- and drug-induced locomotor activity has been clearly demonstrated in adult rats, few studies have evaluated this phenomenon in adolescent rats. In the present study, we determined if the simultaneous exposure to stress and nicotine was capable of inducing behavioral sensitization to nicotine in adolescent and adult rats. To this end, adolescent (postnatal day (P 28-37 and adult (P60-67 rats received nicotine (0.4 mg/kg, sc or saline (0.9% NaCl, sc and were immediately subjected to restraint stress for 2 h once a day for 7 days. The control group for stress was undisturbed following nicotine or saline injections. Three days after the last exposure to stress and nicotine, rats were challenged with a single dose of nicotine (0.4 mg/kg, sc or saline and nicotine-induced locomotion was then recorded for 30 min. In adolescent rats, nicotine caused behavioral sensitization only in animals that were simultaneously exposed to stress, while in adult rats nicotine promoted sensitization independently of stress exposure. These findings demonstrate that adolescent rats are more vulnerable to the effects of stress on behavioral sensitization to nicotine than adult rats.

  3. Rapid and sensitive determination of deuterium concentration by gas chromatography

    International Nuclear Information System (INIS)

    Takahashi, Tomiki; Ohokoshi, Sumio; Shinriki, Nariko; Sato, Toshio

    1984-01-01

    Gas chromatographic determination of hydrogen isotopes D 2 and HD has hitherto been carried out with a molecular sieve column kept at -195 0 C under the H 2 carrier gas. However, the amount of D 2 in hydrogen gas containing low HD concentration of less than 5 % can be practically neglected judging from the equilibrium constant of H 2 -D 2 exchange reaction. Therefore, there is no need to separate HD from D 2 . As an improvement, in this paper, the gas chromatographic determination of HD in low concentration ( 2 as a carrier gas enabled us to enhance the cell current of TCD drastically, hence gave rise to high sensitivity of HD detection. The limit of determination of the concentration of HD was 0.01%. In the case of the higher concentration (>5%) of HD in hydrogen gas, D 2 and HD have been separated and determined by the method described above, but this method takes more than ten minutes. Therefore, we designed a new gas chromatographic analysis of the HD-D 2 mixture with an activated alumina column at -195 0 C under the H 2 carrier gas (330 ml/min). The advantages of this method are in (1) rapid analysis (in 1 min), (2) no need of the rigid activation temperature ((110--250) 0 C), (3) no change of the relative molar sensitivity of HD to D 2 at the various flow rates of H 2 carrier gas ((100--300)ml/min). (author)

  4. Rapidly Simultaneous Determination of Six Effective Components in Cistanche tubulosa by Near Infrared Spectroscopy

    Directory of Open Access Journals (Sweden)

    Xinhong Wang

    2017-05-01

    Full Text Available Quantitative determination of multiple effective components in a given plant usually requires a very large amount of authentic natural products. In this study, we proposed a rapid and non-destructive method for the simultaneous determination of echinacoside, verbascoside, mannitol, sucrose, glucose and fructose in Cistanche tubulosa by near infrared spectroscopy (NIRS. Near infrared diffuse reflectance spectroscopy (DRS and high performance liquid chromatography (HPLC were conducted on 116 batches of C. tubulosa samples. The DRS data were processed using standard normal variety (SNV and multiplicative scatter correction (MSC methods. Partial least squares regression (PLSR was utilized to build calibration models for components-of-interest in C. tubulosa. All models were then assessed by calculating the root mean square error of calibration (RMSEC, correlation coefficient of calibration (r. The r values of all six calibration models were determined to be greater than 0.94, suggesting each model is reliable. Therefore, the quantitative NIR models reported in this study can be qualified to accurately quantify the contents of six medicinal components in C. tubulosa.

  5. Simultaneous HPLC determination of caffeine, theobromine, and theophylline in food, drinks, and herbal products.

    Science.gov (United States)

    Srdjenovic, Branislava; Djordjevic-Milic, Vukosava; Grujic, Nevena; Injac, Rade; Lepojevic, Zika

    2008-02-01

    A rapid and selective high-performance liquid chromatographic (HPLC) method is developed for the separation and determination of caffeine, theobromine, and theophylline. The chromatography is performed on a Zorbax Eclipse XDB-C8 column (4.6x150 mm i.d., 5-microm particle size) at 25 degrees C, with a mobile phase of water-THF (0.1% THF in water, pH 8)-acetonitrile (90:10, v/v). The flow rate is 0.8 mL/min, and detection is by UV at 273 nm. This method permits the simultaneous determination of caffeine, theobromine, and theophylline in food, drinks, and herbal products with detection limits of 0.07-0.2 mg/L and recoveries of 100.20-100.42%. Correlation coefficients, for the calibration curves in the linear range of 0.2-100 mg/L, are greater than 0.9999 for all compounds. The within- and between-day precision is determined for both retention times and peak area. The data suggests that the proposed HPLC method can be used for routine quality control of food, drinks, and herbal products.

  6. Development and validation of an high-performance liquid chromatography-diode array detector method for the simultaneous determination of six phenolic compounds in abnormal savda munziq decoction

    Science.gov (United States)

    Tian, Shuge; Liu, Wenxian; Liu, Feng; Zhang, Xuejia; Upur, Halmuart

    2015-01-01

    Aims: Given the high-effectiveness and low-toxicity of abnormal savda munziq (ASMQ), its herbal formulation has long been used in traditional Uyghur medicine to treat complex diseases, such as cancer, diabetes, and cardiovascular diseases. Settings and Design: ASMQ decoction by reversed-phase high-performance liquid chromatography coupled with a diode array detector was successfully developed for the simultaneous quality assessment of gallic acid, protocatechuic acid, caffeic acid, rutin, rosmarinic acid, and luteolin. The six phenolic compounds were separated on an Agilent TC-C18 reversed-phase analytical column (4.6 × 250 mm, 5 μm) by gradient elution using 0.3% aqueous formic acid (v/v) and 0.3% methanol formic acid (v/v) at 1.0 mL/min. Materials and Methods: The plant material was separately ground and mixed at the following ratios (10): Cordia dichotoma (10.6), Anchusa italic (10.6), Euphorbia humifusa (4.9), Adiantum capillus-veneris (4.9), Ziziphus jujube (4.9), Glycyrrhiza uralensis (7.1), Foeniculum vulgare (4.9), Lavandula angustifolia (4.9), Dracocephalum moldavica L. (4.9), and Alhagi pseudoalhagi (42.3). Statistical Analysis Used: The precisions of all six compounds were Highly significant linear correlations were found between component concentrations and specific chromatographic peak areas (R2 > 0.999). Results: The proposed method was successfully applied to determine the levels of six active components in ASMQ. Conclusions: Given the simplicity, precision, specificity, and sensitivity of the method, it can be utilized as a quality control approach to simultaneously determining the six phenolic compounds in AMSQ. PMID:25709227

  7. Simultaneous determination of short-to-medium lived nuclides in Ghanaian food items using INAA and Compton suppression counting

    International Nuclear Information System (INIS)

    Nyarko, B.J.B.; Fletcher, J.J.; Zwicker, B.; Chatt, A.

    2006-01-01

    An instrumental neutron activation analysis (INAA) method was developed for the simultaneous determination of 19 elements in 10 individual food items from Ghana. The samples were irradiated for 1 minutes in a neutron flux of 2.5 x 10 11 n x cm -2 x s -1 at the Dalhousie University Slowpoke-2 reactor (DUSR) facility. After a 2-minute decay the samples were counted using a Compton suppression gamma-ray spectrometry system for 10 minutes to quantify Ba, Br, Ca, Cl, Co, Cu, Dy, K, Mg, Mn, Na, Rb, S, Sr, Th, Ti, U, V and Zn. The analytical procedure namely, irradiation, decay and counting times were optimized for quick turn-around time for simultaneous determination of the nineteen elements. White-seeded beans (Phaseolus coccineus), one of the most commonly consumed foodstuff in Ghana, were found to contain the highest level of the 19 elements determined, viz. K (1.4%) and Sorghum spp. the lowest level viz. Dy (2.2 ng x g -1 ). Two NIST SRMs were used for internal quality control. The concentrations of most of the elements were found to be within ±6% of the certified or information values. The precisions were calculated from six replicate measurements and were found to be within 10%. (author)

  8. Simultaneous determination of anthraquinones, their 8-beta-D-glucosides, and sennosides of Rhei Rhizoma by capillary electrophoresis.

    Science.gov (United States)

    Koyama, Junko; Morita, Izumi; Fujiyoshi, Hirotaka; Kobayashi, Norihiro

    2005-05-01

    The simultaneous separation and determination of major anthraquinones (emodin, chrysophanol, rhein and their glucosides, aloe-emodin, sennoside A, and sennoside B) of Rhei Rhizoma were achieved by cyclodextrin modified capillary zone electrophoresis. The running electrolyte used in this method was 0.005 M alpha-cyclodextrin in 0.03 M borate buffer (pH 10.0) containing 20% acetonitrile, with an applied voltage of 20 kV.

  9. High-sensitivity simultaneous liquid chromatography-tandem mass spectrometry assay of ethinyl estradiol and levonorgestrel in human plasma

    Institute of Scientific and Technical Information of China (English)

    Abhishek Gandhi; Swati Guttikar; Priti Trivedi

    2015-01-01

    A sensitive and simultaneous liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of ethinyl estradiol and levonorgestrel. The analytes were extracted with methyl-tert-butyl ether: n-hexane (50:50, v/v) solvent mixture, followed by dansyl derivatization. The chromatographic separation was performed on a Kinetex C18 (50 mm × 4.6 mm, 2.6μm) column with a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile in gradient composition. The mass transitions were monitored in electrospray positive ionization mode. The assay exhibited a linear range of 0.100-20.0 ng/mL for levonorgestrel and 4.00-500 pg/mL for ethinyl estradiol in human plasma. A run time of 9.0 min for each sample made it possible to analyze a throughput of more than 100 samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic and bioequivalence studies.

  10. Simultaneous Determination of Ciprofloxacin and Tinidazole in ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, sensitive and specific liquid chromatographic method with PDA ... Conclusion: The developed method is precise, accurate, reproducible and specific and it can .... excel-2007 software and data were considered.

  11. A sensitive fluorescence quenching method for determination of bismuth with tiron

    Energy Technology Data Exchange (ETDEWEB)

    Taher, Mohammad Ali; Rahimi, Mina [Department of Chemistry, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Fazelirad, Hamid, E-mail: hamidfazelirad@gmail.com [Department of Chemistry, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Department of Chemistry, Science and Research Branch, Islamic Azad University, Yazd (Iran, Islamic Republic of); Young Researchers Society, Shahid Bahonar University of Kerman, P.O. Box 76175-133, Kerman (Iran, Islamic Republic of)

    2014-01-15

    We describe a fluorescence quenching method for determination of bismuth with tiron. The method is based on the reaction of tiron by bismuth(III) in acidic media. The influence of variables such as the pH, type of buffer, tiron concentration, reaction time and temperature were investigated. Under optimized conditions, the fluorescence quenching extent is proportional to the concentration of bismuth for Bi–tiron system at the range 0.13–2.09 μg mL{sup −1} and the detection limit is 0.05 μg mL{sup −1}. The proposed sensor presented good repeatability, evaluated in terms of relative standard deviation (R.S.D.=±0.498%) for 11 replicates. This sensitive, rapid and accurate method has been successfully applied to the determination of trace bismuth(III) in water and hair samples and certified reference materials. -- Highlights: • No previous paper report on use of fluorescence quenching for determination of Bi. • Fluorescence quenching of trion is a sensitive method for determination of Bi(III). • Under the optimum conditions the detection limit is very low (0.05 μg mL{sup −1}). • The procedure is simple and safe and has high tolerance limit to interferences.

  12. Simultaneous determination of paracetamol and ibuprofen in pharmaceutical samples by differential pulse voltammetry using a boron-doped diamond electrode

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Amanda B.; Guimaraes, Carlos F.R.C.; Verly, Rodrigo M.; Silva, Leonardo M. da [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil). Departamento de Quimica; Torres, Livia M.F.C.; Carvalho, Junior, Alvaro D.; Santos, Wallans T. P. dos, E-mail: wallanst@ufvjm.edu.br [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil). Departamento de Farmacia

    2014-03-15

    This work presents a simple, fast and low-cost methodology for the simultaneous determination of paracetamol (PC) and ibuprofen (IB) in pharmaceutical formulations by differential pulse voltammetry using a boron-doped diamond (BDD) electrode. A well-defined oxidation peak was observed using the BDD electrode for each analyte (0.85 V for PC and 1.72 V for IB (vs. Ag/AgCl)) in 0.1 mol L{sup -1} H{sub 2}SO{sub 4} solution containing 10% (v/v) of ethanol. Calibration curves for the simultaneous determination of PC and IB showed a linear response for both drugs in a concentration range of 20 to 400 μmol L{sup -1} (r{sup 2} = 0.999), with a detection limit of 7.1 μmol L{sup -1} for PC and 3.8 μmol L{sup -1} for IB. The addition-recovery studies in samples were about 100% and the results were validated by chromatographic methods. (author)

  13. Simultaneous determination of paracetamol and ibuprofen in pharmaceutical samples by differential pulse voltammetry using a boron-doped diamond electrode

    International Nuclear Information System (INIS)

    Lima, Amanda B.; Guimaraes, Carlos F.R.C.; Verly, Rodrigo M.; Silva, Leonardo M. da; Torres, Livia M.F.C.; Carvalho Junior, Alvaro D.; Santos, Wallans T. P. dos

    2014-01-01

    This work presents a simple, fast and low-cost methodology for the simultaneous determination of paracetamol (PC) and ibuprofen (IB) in pharmaceutical formulations by differential pulse voltammetry using a boron-doped diamond (BDD) electrode. A well-defined oxidation peak was observed using the BDD electrode for each analyte (0.85 V for PC and 1.72 V for IB (vs. Ag/AgCl)) in 0.1 mol L -1 H 2 SO 4 solution containing 10% (v/v) of ethanol. Calibration curves for the simultaneous determination of PC and IB showed a linear response for both drugs in a concentration range of 20 to 400 μmol L -1 (r 2 = 0.999), with a detection limit of 7.1 μmol L -1 for PC and 3.8 μmol L -1 for IB. The addition-recovery studies in samples were about 100% and the results were validated by chromatographic methods. (author)

  14. Sensitive determination of D-lactic acid and L-lactic acid in urine by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Henry, H; Marmy Conus, N; Steenhout, P; Béguin, A; Boulat, O

    2012-04-01

    D-lactic acid in urine originates mainly from bacterial production in the intestinal tract. Increased D-lactate excretion as observed in patients affected by short bowel syndrome or necrotizing enterocolitis reflects D-lactic overproduction. Therefore, there is a need for a reliable and sensitive method able to detect D-lactic acid even at subclinical elevation levels. A new and highly sensitive method for the simultaneous determination of L- and D-lactic acid by a two-step procedure has been developed. This method is based on the concentration of lactic acid enantiomers from urine by supported liquid extraction followed by high-performance liquid chromatography-tandem mass spectrometry. The separation was achieved by the use of an Astec Chirobiotic™ R chiral column under isocratic conditions. The calibration curves were linear over the ranges of 2-400 and 0.5-100 µmol/L respectively for L- and D-lactic acid. The limit of detection of D-lactic acid was 0.125 µmol/L and its limit of quantification was 0.5 µmol/L. The overall accuracy and precision were well within 10% of the nominal values. The developed method is suitable for production of reference values in children and could be applied for accurate routine analysis. Copyright © 2011 John Wiley & Sons, Ltd.

  15. Simultaneous determination of dihydrotestosterone and its metabolites in mouse sera by LC-MS/MS with chemical derivatization.

    Science.gov (United States)

    Gorityala, Shashank; Yang, Shuming; Montano, Monica M; Xu, Yan

    2018-07-15

    Androgens play a vital role in prostate cancer development, and their elimination and blockade are essential in the disease management. DHT is the key ligand for androgen receptor (AR) in the prostate. It is locally synthesized from testosterone. In the prostate, DHT is predominantly metabolized to α-diol and β-diol. Recent studies indicate that impaired DHT catabolism is associated with prostate cancer, signifying the necessity of a sensitive quantitative method for the determination of DHT and its metabolites. In this work, an LC-MS/MS method for the simultaneous quantification of DHT and its metabolites was developed and validated. Steroid-free sera were prepared and used for the preparation of sera calibrators and quality controls (QCs). DHT and its metabolites along with their respective stable heavy isotope labeled analytes representing internal standards were first extracted with methyl tertiary-butyl ether (MTBE) and derivatized with picolinic acid (PA). The derivatized analytes were then extracted again with MTBE, dried under nitrogen and reconstituted in the mobile phase (80% methanol and 0.2% formic acid in water). Baseline chromatographic separation of the derivatized analytes was achieved isocratically on XTerra C18 column (2.1 × 100 mm) using the mobile phase at a flow rate of 0.25 mL/min. Quantitation was performed using multiple-reaction-monitoring mode with positive electrospray ionization. The method has calibration ranges from 0.0500 ng/mL to 50.0 ng/mL for DHT and its two metabolites with acceptable assay precision, accuracy, recovery, and matrix factor. It was applied to the determination of DHT and its metabolites in an animal study. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Ligandless, ion pair-based and ultrasound assisted emulsification solidified floating organic drop microextraction for simultaneous preconcentration of ultra-trace amounts of gold and thallium and determination by GFAAS.

    Science.gov (United States)

    Fazelirad, Hamid; Taher, Mohammad Ali

    2013-01-15

    In the present work, a new, simple and efficient method for simultaneous preconcentration of ultra-trace amounts of gold and thallium is developed using an ion pair based-ultrasound assisted emulsification-solidified floating organic drop microextraction procedure before graphite furnace atomic absorption spectrometry determination. This methodology was used to preconcentrate the ion pairs formed between AuCl(4)(-) and TlCl(4)(-) and [C(23)H(42)]N(+) in a microliter-range volume of 1-undecanol. Several factors affecting the microextraction efficiency, such as HCl volume, type and volume of extraction solvent, sonication time, sample volume, temperature, ionic strength and [C(23)H(42)]NCl volume were investigated and optimized. Under the optimized conditions, the enrichment factor of 441 and 443 and calibration graphs of 2.2-89 and 22.2-667 ng L(-1) for gold and thallium were obtained, respectively. The intra- and inter-day precision of ± 4.4 and ± 4.9% for Au and ± 4.8 and ± 5.4% for Tl were obtained. The detection limit was 0.66 ng L(-1) for Au and 4.67 ng L(-1) for Tl. The results show that the liquid-liquid pretreatment using ion pair forming, is sensitive, rapid, simple and safe method for the simultaneous preconcentration of gold and thallium. The method was successfully applied for determination of gold and thallium in natural water and hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Validation of HPLC method for the simultaneous and quantitative determination of 12 UV-filters in cosmetics.

    Science.gov (United States)

    Nyeborg, M; Pissavini, M; Lemasson, Y; Doucet, O

    2010-02-01

    The aim of the study was the validation of a high-performance liquid chromatography (HPLC) method for the simultaneous and quantitative determination of twelve commonly used organic UV-filters (phenylbenzimidazole sulfonic acid, benzophenone-3, isoamyl p-methoxycinnamate, diethylamino hydroxybenzoyl hexyl benzoate, octocrylene, ethylhexyl methoxycinnamate, ethylhexyl salicylate, butyl methoxydibenzoylmethane, diethylhexyl butamido triazone, ethylhexyl triazone, methylene bis-benzotriazolyl tetramethylbutylphenol and bis-ethylhexyloxyphenol methoxyphenyl triazine) contained in suncare products. The separation and quantitative determination was performed in <30 min, using a Symmetry Shield(R) C18 (5 microm) column from Waters and a mobile phase (gradient mode) consisting of ethanol and acidified water. UV measurements were carried out at multi-wavelengths, according to the absorption of the analytes.

  18. [Simultaneous determination of amlodipine, benazepril and benazeprilat in human plasma by LC-HESI/MS/MS method].

    Science.gov (United States)

    Pan, Hua-Ling; Lin, Li-Shan; Ding, Jue-Fang; Chen, Xiao-Yan; Zhong, Da-Fang

    2014-01-01

    The study aims to develop a rapid, sensitive and specified method of liquid chromatography with heated electrospray ionization tandem mass spectrometry (LC-HESI/MS/MS) for simultaneous determination of amlodipine, benazepril and benazeprilat in human plasma using amlodipine-d4 and ubenimex as internal standards (ISs). Selected reaction monitoring (SRM) with heated electrospray ionization (HESI) was used in the positive mode for mass spectrometric detection. Analytes and ISs were extracted from plasma by simple protein precipitation. The reconstituted samples were chromatographed on a C18 (100 mm x 4.6 mm, 5 microm) column with mixture of methanol-acetonitrile-5 mmol.L- ammonium acetate-formic acid (30 : 30 : 40 : 0.1) as mobile phase at a flow rate of 0.6 mL.min-1. The standard curves were demonstrated to be linear in the range of 0.02 to 6.00 ng.mL-1 for amlodipine, 0.2 to 1,500 ng.mL-1 for benazepril and benazeprilat with r2>0.99 for each analyte. The lower limit of quantitation was identifiable and reproducible at 0.02, 0.2 and 0.2 ng mL-1 for amlodipine, benazepril and benazeprilat, respectively. The intra-day and inter-day precision and accuracy results were within the acceptable limit across all concentrations. The plasma samples were stable after four freeze-thaw cycles and being stored for 93 days at -20 degrees C. The method was applied to a pharmacokinetic study of a fixed-dose combination of amlodipine and benazepril on Chinese healthy volunteers.

  19. Radioactivity measurements for determining bacterial increase and sensitivity to antibiotics. [/sup 14/C tracer

    Energy Technology Data Exchange (ETDEWEB)

    Jaszsagi-Nagy, E [Magyar Tudomanyos Akademia, Budapest; Lendvay, J [Orszagos Frederic Joliot-Curie Sugarbiologiai es Sugaregeszsegugyi Kutato Intezet, Budapest (Hungary)

    1976-01-01

    The authors elaborated a sensitive and objective measuring method for determining the bacteria increase in biological material and the sensitivity to antibiotics. When /sup 14/C glucose is added to the medium as the single source of sugar, the respiratory carbon dioxide formed by the bacteria reflects the rate of increase. The released /sup 14/C dioxide can be measured continuously without loss to the environment and the degree of bacterial infection and the antibiotic activity, respectively, can be determined.

  20. Multiplexed Simultaneous High Sensitivity Sensors with High-Order Mode Based on the Integration of Photonic Crystal 1 × 3 Beam Splitter and Three Different Single-Slot PCNCs

    Directory of Open Access Journals (Sweden)

    Jian Zhou

    2016-07-01

    Full Text Available We simulated an efficient method for the sensor array of high-sensitivity single-slot photonic crystal nanobeam cavities (PCNCs on a silicon platform. With the combination of a well-designed photonic crystal waveguide (PhCW filter and an elaborate single-slot PCNC, a specific high-order resonant mode was filtered for sensing. A 1 × 3 beam splitter carefully established was implemented to split channels and integrate three sensors to realize microarrays. By applying the three-dimensional finite-difference-time-domain (3D-FDTD method, the sensitivities calculated were S1 = 492 nm/RIU, S2 = 244 nm/RIU, and S3 = 552 nm/RIU, respectively. To the best of our knowledge, this is the first multiplexing design in which each sensor cite features such a high sensitivity simultaneously.

  1. STIS E140M Sensitivity Curves

    Science.gov (United States)

    Monroe, TalaWanda R.

    2017-08-01

    The spectrophotometric white dwarf G191-B2B will be observed with the E140M grating to obtain an updated set of sensitivity curves for this highly used mode. Spectroscopic sensitivity monitoring observations of BD+284211 have shown that the blaze function shapes have changed since SM4 and now limit the relative photometric flux accuracy of 14 of 43 E140M spectral orders to 5-10% at the edges. The blaze function shape changes have hindered attempts to determine the post-SM4 temporal blaze function shifts for this grating. Given the popularity of this unique FUV mode, with almost full simultaneous coverage of 1144 to 1710 A in a single observation, and consideration of the STIS archival legacy, we request 1 orbit to re-observe G191-B2B with the E140/1425 setting.

  2. Simultaneous determination of umbelliferone and scopoletin in Tibetan medicine Saussurea laniceps and traditional Chinese medicine Radix angelicae pubescentis using excitation-emission matrix fluorescence coupled with second-order calibration method

    Science.gov (United States)

    Wang, Li; Wu, Hai-Long; Yin, Xiao-Li; Hu, Yong; Gu, Hui-Wen; Yu, Ru-Qin

    2017-01-01

    A chemometrics-assisted excitation-emission matrix (EEM) fluorescence method is presented for simultaneous determination of umbelliferone and scopoletin in Tibetan medicine Saussurea laniceps (SL) and traditional Chinese medicine Radix angelicae pubescentis (RAP). Using the strategy of combining EEM fluorescence data with second-order calibration method based on the alternating trilinear decomposition (ATLD) algorithm, the simultaneous quantification of umbelliferone and scopoletin in the two different complex systems was achieved successfully, even in the presence of potential interferents. The pretreatment is simple due to the "second-order advantage" and the use of "mathematical separation" instead of awkward "physical or chemical separation". Satisfactory results have been achieved with the limits of detection (LODs) of umbelliferone and scopoletin being 0.06 ng mL- 1 and 0.16 ng mL- 1, respectively. The average spike recoveries of umbelliferone and scopoletin are 98.8 ± 4.3% and 102.5 ± 3.3%, respectively. Besides, HPLC-DAD method was used to further validate the presented strategy, and t-test indicates that prediction results of the two methods have no significant differences. Satisfactory experimental results imply that our method is fast, low-cost and sensitive when compared with HPLC-DAD method.

  3. Simultaneous determination of seven flavonoids in Epimedium by liquid chromatography-tandem mass spectrometry method

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Bao Lin Guo; Yu Xin Sheng; Jin Lan Zhang

    2008-01-01

    In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2"-0-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.

  4. Morphology-dependent Electrochemical Enhancements of Porous Carbon as Sensitive Determination Platform for Ascorbic Acid, Dopamine and Uric Acid

    Science.gov (United States)

    Cheng, Qin; Ji, Liudi; Wu, Kangbing; Zhang, Weikang

    2016-02-01

    Using starch as the carbon precursor and different-sized ZnO naoparticles as the hard template, a series of porous carbon materials for electrochemical sensing were prepared. Experiments of scanning electron microscopy, transmission electron microscopy and Nitrogen adsorption-desorption isotherms reveal that the particle size of ZnO has big impacts on the porous morphology and surface area of the resulting carbon materials. Through ultrasonic dispersion of porous carbon and subsequent solvent evaporation, different sensing interfaces were constructed on the surface of glassy carbon electrode (GCE). The electrochemical behaviors of ascorbic acid (AA), dopamine (DA) and uric acid (UA) were studied. On the surface of porous carbon materials, the accumulation efficiency and electron transfer ability of AA, DA and UA are improved, and consequently their oxidation signals enhance greatly. Moreover, the interface enhancement effects of porous carbon are also controlled by the particle size of hard template. The constructed porous carbon interface displays strong signal amplification ability and holds great promise in constructing a sensitive platform for the simultaneous determination of AA, DA and UA.

  5. Simultaneous determination of arsenic, selenium and antimony species using HPLC/ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Lindemann, T.; Prange, A.; Neidhart, B. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Physikalische und Chemische Analytik; Dannecker, W. [Univ. of Hamburg (Germany). Inst. for Inorganic and Applied Chemistry

    1999-07-01

    A new method for the simultaneous separation and determination of four arsenic species [As(III), As(V), monomethylarsonic acid and dimethylarsinic acid], three selenium species [Se(IV), Se(VI) and selenomethionine] as well as Sb(III) and Sb(V) is presented. The speciation was achieved by on-line coupling of anion exchange high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic parameters such as the composition and pH of the mobile phase were optimised. Limits of detection are below 4.5 {mu}g L{sup -1} (as element) for Sb(III) and the selenium species and below 0.5 {mu}g L{sup -1} for the other species. Precisions of retention times were better than 2% RSD and of peak areas better than 8% RSD for all the species investigated. (orig.) With 5 figs., 3 tabs., 41 refs.

  6. Effects of simultaneous exposure to stress and nicotine on nicotine-induced locomotor activation in adolescent and adult rats

    Energy Technology Data Exchange (ETDEWEB)

    Zago, A. [Laboratório de Farmacologia, Faculdade de Ciências Farmacêuticas, Universidade Estadual Paulista, Araraquara, SP (Brazil); Leão, R.M.; Carneiro-de-Oliveira, P.E. [Laboratório de Farmacologia, Faculdade de Ciências Farmacêuticas, Universidade Estadual Paulista, Araraquara, SP (Brazil); Programa Interinstitucional de Pós-Graduação em Ciências Fisiológicas, Universidade Federal de São Carlos/Universidade Estadual de São Paulo, Araraquara, SP (Brazil); Marin, M.T.; Cruz, F.C. [Laboratório de Farmacologia, Faculdade de Ciências Farmacêuticas, Universidade Estadual Paulista, Araraquara, SP (Brazil); Planeta, C.S. [Laboratório de Farmacologia, Faculdade de Ciências Farmacêuticas, Universidade Estadual Paulista, Araraquara, SP (Brazil); Programa Interinstitucional de Pós-Graduação em Ciências Fisiológicas, Universidade Federal de São Carlos/Universidade Estadual de São Paulo, Araraquara, SP (Brazil)

    2011-11-18

    Preclinical studies have shown that repeated stress experiences can result in an increase in the locomotor response to the subsequent administration of drugs of abuse, a phenomenon that has been termed behavioral cross-sensitization. Behavioral sensitization reflects neuroadaptive processes associated with drug addiction and drug-induced psychosis. Although crosssensitization between stress- and drug-induced locomotor activity has been clearly demonstrated in adult rats, few studies have evaluated this phenomenon in adolescent rats. In the present study, we determined if the simultaneous exposure to stress and nicotine was capable of inducing behavioral sensitization to nicotine in adolescent and adult rats. To this end, adolescent (postnatal day (P) 28-37) and adult (P60-67) rats received nicotine (0.4 mg/kg, sc) or saline (0.9% NaCl, sc) and were immediately subjected to restraint stress for 2 h once a day for 7 days. The control group for stress was undisturbed following nicotine or saline injections. Three days after the last exposure to stress and nicotine, rats were challenged with a single dose of nicotine (0.4 mg/kg, sc) or saline and nicotine-induced locomotion was then recorded for 30 min. In adolescent rats, nicotine caused behavioral sensitization only in animals that were simultaneously exposed to stress, while in adult rats nicotine promoted sensitization independently of stress exposure. These findings demonstrate that adolescent rats are more vulnerable to the effects of stress on behavioral sensitization to nicotine than adult rats.

  7. Effects of simultaneous exposure to stress and nicotine on nicotine-induced locomotor activation in adolescent and adult rats

    International Nuclear Information System (INIS)

    Zago, A.; Leão, R.M.; Carneiro-de-Oliveira, P.E.; Marin, M.T.; Cruz, F.C.; Planeta, C.S.

    2011-01-01

    Preclinical studies have shown that repeated stress experiences can result in an increase in the locomotor response to the subsequent administration of drugs of abuse, a phenomenon that has been termed behavioral cross-sensitization. Behavioral sensitization reflects neuroadaptive processes associated with drug addiction and drug-induced psychosis. Although crosssensitization between stress- and drug-induced locomotor activity has been clearly demonstrated in adult rats, few studies have evaluated this phenomenon in adolescent rats. In the present study, we determined if the simultaneous exposure to stress and nicotine was capable of inducing behavioral sensitization to nicotine in adolescent and adult rats. To this end, adolescent (postnatal day (P) 28-37) and adult (P60-67) rats received nicotine (0.4 mg/kg, sc) or saline (0.9% NaCl, sc) and were immediately subjected to restraint stress for 2 h once a day for 7 days. The control group for stress was undisturbed following nicotine or saline injections. Three days after the last exposure to stress and nicotine, rats were challenged with a single dose of nicotine (0.4 mg/kg, sc) or saline and nicotine-induced locomotion was then recorded for 30 min. In adolescent rats, nicotine caused behavioral sensitization only in animals that were simultaneously exposed to stress, while in adult rats nicotine promoted sensitization independently of stress exposure. These findings demonstrate that adolescent rats are more vulnerable to the effects of stress on behavioral sensitization to nicotine than adult rats

  8. Technical note: Simultaneous carotenoid and vitamin analysis of milk from total mixed ration-fed cows optimized for xanthophyll detection.

    Science.gov (United States)

    Stout, M A; Benoist, D M; Drake, M A

    2018-06-01

    Concentrations of retinol, α-tocopherol, and major carotenoids in dairy products are often determined simultaneously by liquid chromatography. These compounds have different polarity and solubility; thus, extracting them simultaneously can be difficult and inefficient. In milks with low carotenoid concentrations, the xanthophylls lutein and zeaxanthin may not be completely resolved using common extraction techniques. A simplified method was developed to optimize extraction efficiency and the limit of detection and limit of quantification (LoQ) of lutein and zeaxanthin in bovine milk without decreasing sensitivity to other vitamins or carotenoids. The developed method evaluates lutein, zeaxanthin, β-carotene, retinol, and α-tocopherol simultaneously by ultra-high performance liquid chromatography-photodiode array detection. Common saponification temperatures (40-60°C) and concentrations of KOH in water (10-50% KOH wt/vol) were evaluated. Multiple solvents were evaluated for optimal xanthophyll extraction (diethyl ether, dichloromethane, hexane, and tetrahydrofuran) following saponification. The limit of detection and LoQ were defined as 3:1 and 10:1 signal-to-noise ratio, respectively. All experiments were performed in triplicate. The optimal saponification procedure was a concentration of 25% KOH at either 40 or 50°C. Saponified extracts solubilized in solutions containing diethyl ether had greater concentrations of lutein- than hexane- or tetrahydrofuran-based solutions, with peak areas above LoQ values. The solution containing diethyl ether solubilized similar concentrations of retinol, α-tocopherol, and β-carotene when compared with other solutions. The proposed optimized method allows for the simultaneous determination of carotenoids from milk with increased lutein and zeaxanthin sensitivity without sacrificing recovery of retinol, α-tocopherol, and β-carotene. Copyright © 2018 American Dairy Science Association. Published by Elsevier Inc. All rights

  9. Determination of aerodynamic sensitivity coefficients based on the three-dimensional full potential equation

    Science.gov (United States)

    Elbanna, Hesham M.; Carlson, Leland A.

    1992-01-01

    The quasi-analytical approach is applied to the three-dimensional full potential equation to compute wing aerodynamic sensitivity coefficients in the transonic regime. Symbolic manipulation is used to reduce the effort associated with obtaining the sensitivity equations, and the large sensitivity system is solved using 'state of the art' routines. Results are compared to those obtained by the direct finite difference approach and both methods are evaluated to determine their computational accuracy and efficiency. The quasi-analytical approach is shown to be accurate and efficient for large aerodynamic systems.

  10. Simultaneous in vivo determination of calcium and phosphate effective intestinal absorption in the rat

    International Nuclear Information System (INIS)

    Ladizesky, M.; Mautalen, C.A.; Cabrejas, M.; Degrossi, O.J.

    1978-01-01

    A description is given of a technique which allows a more precise assessment of the interrelation between calcium and phosphate transport systems. Rats were given an i.p. or oral dose of 47 Ca with 40 Ca as carrier and/or 32 P with 31 P as carrier. The animals were sacrificed and activities in body and excised gastrointestinal tract determined. The 1.28 MeV photopeak activity was measured for calcium 47, and phosphorus 32 activity was determined by measuring the Bremsstrahlung produced by this isotope in the rat's body in the 80 to 200 keV range. The rates of intestinal absorption of calcium and phosphate differed; there seemed to be no urinary excretion of the radioisotopes within 3 hours. The reciprocal influence of calcium and phosphate on the intestinal absorption was also studied. The technique is simple and allows the simultaneous in vivo measurement of the effective intestinal absorption of calcium and phosphate. (U.K.)

  11. Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake.

    Science.gov (United States)

    Cepeda-Vázquez, Mayela; Blumenthal, David; Camel, Valérie; Rega, Barbara

    2017-03-01

    Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R 2 : 0.9957 for furan and 0.9996 for furfural), LOD (0.50ng furan g sample dry basis -1 and 10.2ng furfural g sample dry basis -1 ), LOQ (0.99ng furan g sample dry basis -1 and 41.1ng furfural g sample dry basis -1 ). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes. Copyright © 2016. Published by Elsevier B.V.

  12. Simultaneous determination of phenolic compounds and saponins in quinoa (Chenopodium quinoa Willd) by a liquid chromatography-diode array detection-electrospray ionization-time-of-flight mass spectrometry methodology.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto; Caboni, Maria Fiorenza

    2011-10-26

    A new liquid chromatography methodology coupled to a diode array detector and a time-of-flight mass spectrometer has been developed for the simultaneous determination of phenolic compounds and saponins in quinoa (Chenopodium quinoa Willd). This method has allowed the simultaneous determination of these two families of compounds with the same analytical method for the first time. A fused-core column C18 has been used, and the analysis has been performed in less than 27 min. Both chromatographic and electrospray ionization time-of-flight mass spectrometry parameters have been optimized to improve the sensitivity and to maximize the number of compounds detected. A validation of the method has also been carried out, and free and bound polar fractions of quinoa have been studied. Twenty-five compounds have been tentatively identified and quantified in the free polar fraction, while five compounds have been tentatively identified and quantified in the bound polar fraction. It is important to highlight that 1-O-galloyl-β-D-glucoside, acacetin, protocatechuic acid 4-O-glucoside, penstebioside, ethyl-m-digallate, (epi)-gallocatechin, and canthoside have been tentatively identified for the first time in quinoa. Free phenolic compounds have been found to be in the range of 2.746-3.803 g/kg of quinoa, while bound phenolic compounds were present in a concentration that varies from 0.139 and 0.164 g/kg. Indeed, saponins have been found to be in a concentration that ranged from 5.6 to 7.5% of the total composition of whole quinoa flour.

  13. Flow injection electrochemical hydride generation inductively coupled plasma time-of-flight mass spectrometry for the simultaneous determination of hydride forming elements and its application to the analysis of fresh water samples

    International Nuclear Information System (INIS)

    Bings, Nicolas H.; Stefanka, Zsolt; Mallada, Sergio Rodriguez

    2003-01-01

    A flow injection (FI) method was developed using electrochemical hydride generation (EcHG) as a sample introduction system, coupled to an inductively coupled plasma time-of-flight mass spectrometer (ICP-TOFMS) for rapid and simultaneous determination of six elements forming hydrides (As, Bi, Ge, Hg, Sb and Se). A novel low volume electrolysis cell, especially suited for FI experiments was designed and the conditions for simultaneous electrochemical hydride generation (EcHG; electrolyte concentrations and flow rates, electrolysis voltage and current) as well as the ICP-TOFMS operational parameters (carrier gas flow rate, modulation pulse width (MPW)) for the simultaneous determination of 12 isotopes were optimized. The compromise operation parameters of the electrolysis were found to be 1.4 and 3 ml min -1 for the anolyte and catholyte flow rates, respectively, using 2 M sulphuric acid. An optimum electrolysis current of 0.7 A (16 V) and an argon carrier gas flow rate of 0.91 l min -1 were chosen. A modulation pulse width of 5 μs, which influences the sensitivity through the amount of ions being collected by the MS per single analytical cycle, provided optimum results for the detection of transient signals. The achieved detection limits were compared with those obtained by using FI in combination with conventional nebulization (FI-ICP-TOFMS); values for chemical hydride generation (FI-CHG-ICP-TOFMS) were taken from the literature. By using a 200 μl sample loop absolute detection limits (3σ) in the range of 10-160 pg for As, Bi, Ge, Hg, Sb and 1.1 ng for Se and a precision of 4-8% for seven replicate injections of 20-100 ng ml -1 multielemental sample solutions were achieved. The analysis of a standard reference material (SRM) 1643d (NIST, 'Trace Elements in Water') showed good agreement with the certified values for As and Sb. Se showed a drastic difference, which is probably due to the presence of hydride-inactive Se species in the sample. Recoveries better than

  14. Simultaneous Determination of Seven Phenolic Acids in Rat Plasma Using UHPLC-ESI-MS/MS after Oral Administration of Echinacea purpurea Extract

    Directory of Open Access Journals (Sweden)

    Yan Du

    2017-09-01

    Full Text Available A rapid and sensitive Ultra High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry (UHPLC-ESI-MS/MS method was developed and validated to simultaneously determine the concentration of seven phenolic acids (syringic acid, ferulic acid, caffeic acid, vanillic acid, p-coumaric acid, 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid in rat plasma after oral administration of Echinacea purpurea extract. After mixing with the internal standard (IS, butylparaben, plasma samples were prepared by liquid–liquid extraction with ethyl acetate. The separation was performed using the Agilent Eclipse Plus C18 column (1.8 μm, 2.1 mm × 50 mm with a gradient system consisting of solution A (0.1% acetic acid in water and solution B (methanol at a flow rate of 0.3 mL/min. The detection was accomplished by a multiple reaction monitoring (MRM mode with electrospray ionization (ESI. The method was validated in terms of linearity, precision, accuracy, extraction recovery, matrix effect and stability. This method was successfully applied to study the pharmacokinetic properties of the seven compounds after oral administration of Echinacea purpurea extract in rats.

  15. Hessian matrix approach for determining error field sensitivity to coil deviations

    Science.gov (United States)

    Zhu, Caoxiang; Hudson, Stuart R.; Lazerson, Samuel A.; Song, Yuntao; Wan, Yuanxi

    2018-05-01

    The presence of error fields has been shown to degrade plasma confinement and drive instabilities. Error fields can arise from many sources, but are predominantly attributed to deviations in the coil geometry. In this paper, we introduce a Hessian matrix approach for determining error field sensitivity to coil deviations. A primary cost function used for designing stellarator coils, the surface integral of normalized normal field errors, was adopted to evaluate the deviation of the generated magnetic field from the desired magnetic field. The FOCUS code (Zhu et al 2018 Nucl. Fusion 58 016008) is utilized to provide fast and accurate calculations of the Hessian. The sensitivities of error fields to coil displacements are then determined by the eigenvalues of the Hessian matrix. A proof-of-principle example is given on a CNT-like configuration. We anticipate that this new method could provide information to avoid dominant coil misalignments and simplify coil designs for stellarators.

  16. Simultaneous determination of amino acids and carbohydrates in culture media of Clostridium thermocellum by valve-switching ion chromatography.

    Science.gov (United States)

    Fa, Yun; Yang, Haiyan; Ji, Chengshuai; Cui, He; Zhu, Xinshu; Du, Juan; Gao, Jun

    2013-10-10

    An improved method for the simultaneous determination of 20 amino acids and 7 carbohydrates using one-valve switching after injection, ion chromatography, and integrated pulsed amperometric detection is proposed. The resolution of the amino acids and carbohydrates in the cation trap column was investigated. In addition, parameters including flow liquid type, flow rate, concentration, and valve-switch timing were optimized. The method is time-saving, effective, and accurate for the simultaneous separation of amino acids and carbohydrates, with a mean correlation coefficient of >0.99 and repeatability of 0.5-4.6% for eight replicates. The method was successfully applied in the analysis of amino acids and carbohydrates in aseptic media and in extracellular culture media of three phenotypes of Clostridium thermocellum. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. A pre-anodized inlaying ultrathin carbon paste electrode for simultaneous determination of uric acid and folic acid

    International Nuclear Information System (INIS)

    Huo, Jing’e; Shangguan, Enbo; Li, Quanmin

    2013-01-01

    Graphical abstract: In 0.10 mol/L PBS (pH 6.00), oxidation reaction occurred at the PAIUCPE owing to uric acid (UA) loss electrons, while oxygen dissolved in the feed was reduced at the platinum electrode. Furthermore, the effect of electrode reaction at the platinum electrode on that of working electrode is detailedly discussed. Highlights: ► The simultaneous determination of UA and FA is achieved at the PAIUCPE. ► The effect of reaction at the Pt electrode on that of working electrode is discussed. ► The effect of pH on peak currents is detailedly explained for the first time. -- Abstract: A pre-anodized inlaying ultrathin carbon paste electrode (PAIUCPE) was prepared by electrochemical pretreatment. The scanning electron microscope (SEM) was applied to characterize the surface morphology of PAIUCPE and the performance of the electrode was characterized by cyclic voltammetry (CV). The results indicated that PAIUCPE displayed excellent electrocatalysis for the oxidation of uric acid (UA) and folic acid (FA). The separated extent between the two oxidation peaks of UA and FA was 324 mV, which was enough for the simultaneous detection. In 0.10 mol/L PBS (pH 6.00), the linear scan voltammetry (LSV) response of UA and FA increased linearly with the concentration in the range of 4.0 × 10 −6 –3.5 × 10 −4 mol/L and 3.0 × 10 −6 –2.0 × 10 −4 mol/L with the detection limits of 1.1 × 10 −7 mol/L and 1.5 × 10 −7 mol/L, respectively. It was successfully used to determine UA and FA in human urine simultaneously

  18. A rapid simultaneous determination of methylxanthines and proanthocyanidins in Brazilian guaraná (Paullinia cupana Kunth.).

    Science.gov (United States)

    Machado, Kamilla Nunes; Freitas, Aline Alves de; Cunha, Luzia Helena; Faraco, André Augusto Gomes; Pádua, Rodrigo Maia de; Braga, Fernão Castro; Vianna-Soares, Cristina Duarte; Castilho, Rachel Oliveira

    2018-01-15

    Paullinia cupana is a plant native to Brazil that is widely used in traditional medicine as a physical and mental stimulant. It is also used worldwide to produce soft drinks. A method for the simultaneous quantitation of seven markers in guaraná by HPLC-PDA was developed, and extraction methods for the determination of methylxanthines and tannins were investigated. Quantified substances were theobromine, theophylline, caffeine, catechin, epicatechin, procyanidins A2 and B2. Results confirmed the satisfactory selectivity and linearity (r 2 ≥0.99) within the mass ranges. Repeatability (RSD≤2.80%), intermediate precision (RSD≤4.47%), accuracy (recoveries from 90.59%-104.67%), and robustness were demonstrated. Extract 1 presented the contents: 0.0177% (±1.02%) for theobromine, 0.0131% (±1.14%) for theophylline, 2.9429% (±1.27%) for caffeine, 0.4563% (±1.02%) for catechin, 0.5515% (±1.05%) for epicatechin, 0.0607% (±2.80%) for A2 and 0.1035% (±1.39%) for B2. The method for simultaneous quantitation of seven chemical markers in guaraná proved to be reliable using a simple and convenient HPLC setup. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Multiplex Real-Time qPCR Assay for Simultaneous and Sensitive Detection of Phytoplasmas in Sesame Plants and Insect Vectors.

    Directory of Open Access Journals (Sweden)

    Cengiz Ikten

    Full Text Available Phyllody, a destructive and economically important disease worldwide caused by phytoplasma infections, is characterized by the abnormal development of floral structures into stunted leafy parts and contributes to serious losses in crop plants, including sesame (Sesamum indicum L.. Accurate identification, differentiation, and quantification of phyllody-causing phytoplasmas are essential for effective management of this plant disease and for selection of resistant sesame varieties. In this study, a diagnostic multiplex qPCR assay was developed using TaqMan® chemistry based on detection of the 16S ribosomal RNA gene of phytoplasmas and the 18S ribosomal gene of sesame. Phytoplasma and sesame specific primers and probes labeled with different fluorescent dyes were used for simultaneous amplification of 16SrII and 16SrIX phytoplasmas in a single tube. The multiplex real-time qPCR assay allowed accurate detection, differentiation, and quantification of 16SrII and 16SrIX groups in 109 sesame plant and 92 insect vector samples tested. The assay was found to have a detection sensitivity of 1.8 x 102 and 1.6 x 102 DNA copies for absolute quantification of 16SrII and 16SrIX group phytoplasmas, respectively. Relative quantification was effective and reliable for determination of phyllody phytoplasma DNA amounts normalized to sesame DNA in infected plant tissues. The development of this qPCR assay provides a method for the rapid measurement of infection loads to identify resistance levels of sesame genotypes against phyllody phytoplasma disease.

  20. A Validated Stability-Indicating HPLC Method for Simultaneous Determination of Amoxicillin and Enrofloxacin Combination in an Injectable Suspension

    Directory of Open Access Journals (Sweden)

    Nidal Batrawi

    2017-02-01

    Full Text Available The combination of amoxicillin and enrofloxacin is a well-known mixture of veterinary drugs; it is used for the treatment of Gram-positive and Gram-negative bacteria. In the scientific literature, there is no high-performance liquid chromatography (HPLC-UV method for the simultaneous determination of this combination. The objective of this work is to develop and validate an HPLC method for the determination of this combination. In this regard, a new, simple and efficient reversed-phase HPLC method for simultaneous qualitative and quantitative determination of amoxicillin and enrofloxacin, in an injectable preparation with a mixture of inactive excipients, has been developed and validated. The HPLC separation method was performed using a reversed-phase (RP-C18e (250 mm × 4.0 mm, 5 μm column at room temperature, with a gradient mobile phase of acetonitrile and phosphate buffer containing methanol at pH 5.0, a flow rate of 0.8 mL/min and ultraviolet detection at 267 nm. This method was validated in accordance with the Food and Drug Administration (FDA and the International Conference on Harmonisation (ICH guidelines and showed excellent linearity, accuracy, precision, specificity, robustness, ruggedness, and system suitability results within the acceptance criteria. A stability-indicating study was also carried out and indicated that this method can also be used for purity and degradation evaluation of these formulations.

  1. Derivative spectrophotometric method for simultaneous determination of clindamycin phosphate and tretinoin in pharmaceutical dosage forms.

    Science.gov (United States)

    Barazandeh Tehrani, Maliheh; Namadchian, Melika; Fadaye Vatan, Sedigheh; Souri, Effat

    2013-04-10

    A derivative spectrophotometric method was proposed for the simultaneous determination of clindamycin and tretinoin in pharmaceutical dosage forms. The measurement was achieved using the first and second derivative signals of clindamycin at (1D) 251 nm and (2D) 239 nm and tretinoin at (1D) 364 nm and (2D) 387 nm.The proposed method showed excellent linearity at both first and second derivative order in the range of 60-1200 and 1.25-25 μg/ml for clindamycin phosphate and tretinoin respectively. The within-day and between-day precision and accuracy was in acceptable range (CVpharmaceutical dosage form.

  2. Validated assay for the simultaneous quantification of total vincristine and actinomycin-D concentrations in human EDTA plasma and of vincristine concentrations in human plasma ultrafiltrate by high-performance liquid chromatography coupled with tandem mass spectrometry

    NARCIS (Netherlands)

    Damen, Carola W. N.; Israëls, Trijn; Caron, Huib N.; Schellens, Jan H. M.; Rosing, Hilde; Beijnen, Jos H.

    2009-01-01

    A sensitive, specific and efficient high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) assay for the simultaneous determination of total vincristine and actinomycin-D concentrations in human plasma and an assay for the determination of unbound vincristine are presented.

  3. A new innovative spectrophotometric method for the simultaneous determination of sofosbuvir and ledipasvir

    Science.gov (United States)

    Mansour, Fotouh R.

    2018-01-01

    A new innovative spectrophotometric method is developed to determine the concentration ratios in binary mixtures by determining the zero crossing point in the first derivative of the gross curve. This relationship can be applied if the part of the UV spectrum of substance Y, that intersects with the overlaid spectra of substance X is straight. By plotting the intersection wavelength against the concentration ratio (Cx/Cy), a straight line was obtained with a co-efficient of determination equals 0.9999. As an application, simultaneous determination of sofosbuvir and ledipasvir in their binary mixtures was performed using two methods; a direct UV spectrophotometric method for determination of ledipasvir at 333 nm, and the new "wavelength-intersection ratio" method for determination of sofosbuvir. In the wavelength-intersection ratio method, different mixtures of sofosbuvir and ledipasvir containing different concentration ratios were prepared; the zero crossing point of the first derivative curve in the range 285 to 295 nm were determined for each mixture. An absorbance shift in the intersection was obtained with the change in the concentration ratio (sofosbuvir/ledipasvir). When the concentration ratio was plotted against the intersection wavelength, a straight line was obtained with a coefficient of determination of 0.9992. The direct method was linear in the range 3 to 18 μg/mL while the wavelength-intersection ratio method was linear in the range 11-110 μg/mL. The limits of detection were determined and found to be 0.5 and 3 μg/mL for ledipasvir and sofosbuvir, respectively. The accuracy and repeatability of the two methods were tested. The mean %recovery was found to be 100.19% and 100.75% for ledipasvir and sofosbuvir, respectively. The relative standard deviation was 0.57 for ledipasvir and 1.79 for sofosbuvir. The intermediate precision was also checked, the coefficients of variation for sofosbuvir and ledipasvir measurements between days did not exceed 1.88%.

  4. An improved experimental scheme for simultaneous measurement of high-resolution zero electron kinetic energy (ZEKE) photoelectron and threshold photoion (MATI) spectra

    Science.gov (United States)

    Michels, François; Mazzoni, Federico; Becucci, Maurizio; Müller-Dethlefs, Klaus

    2017-10-01

    An improved detection scheme is presented for threshold ionization spectroscopy with simultaneous recording of the Zero Electron Kinetic Energy (ZEKE) and Mass Analysed Threshold Ionisation (MATI) signals. The objective is to obtain accurate dissociation energies for larger molecular clusters by simultaneously detecting the fragment and parent ion MATI signals with identical transmission. The scheme preserves an optimal ZEKE spectral resolution together with excellent separation of the spontaneous ion and MATI signals in the time-of-flight mass spectrum. The resulting improvement in sensitivity will allow for the determination of dissociation energies in clusters with substantial mass difference between parent and daughter ions.

  5. A novel magnetic ionic liquid modified carbon nanotube for the simultaneous determination of aryloxyphenoxy-propionate herbicides and their metabolites in water

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Mai; Liu, Donghui; Zhao, Lu; Han, Jiajun; Liang, Yiran; Wang, Peng; Zhou, Zhiqiang, E-mail: zqzhou@cau.edu.cn

    2014-12-10

    Highlights: • A new kind of ionic liquid modified carbon nanotube has been synthesized and applied for simultaneous analysis of AOPPs and their metabolites. • The potential pollutants, such as metabolites of AOPPs, have been analyzed. • The mechanism of absorption has been discussed. • Varieties of experiment factors were optimized and selected. • This method has been successfully applied in the analysis of real water samples. - Abstract: A reliable, sensitive, rapid and environmentally friendly analysis procedure for the simultaneous determination of the analytes with a wide range of polarity in the environmental water was developed by coupling dispersive magnetic solid-phase extraction (d-MSPE) with high-performance liquid chromatography (HPLC)–diode array detector (DAD) and ultra-high pressure liquid chromatography (UHPLC)-triple quadrupole mass spectrometer (MS/MS), in this work. Magnetic ionic liquid modified multi-walled carbon nanotubes (m-IL-MWCNTs) were prepared by spontaneous assembly of magnetic nanoparticles and imidazolium-modified carbon nanotubes, and used as the sorbent of d-MSPE to simultaneously extract aryloxyphenoxy-propionate herbicides (AOPPs) and their polar acid metabolites due to the excellent π–π electron donor–acceptor interactions and anion exchange ability. The factors, including the amount of sorbent, pH of the sample solution, extraction time and the volume of elution solvent were investigated. Under the optimized conditions, the proposed d-MSPE coupling to HPLC–DAD system had a satisfactory performance, the limits of detection (LODs, defined as the signal to noise ratio of 3) and the limits of quantification (LOQs, defined as the signal to noise ratio of 10) for analytes in Milli-Q water were in the range of 2.8–14.3 and 9.8–43.2 μg L{sup −1} respectively. Calibration curves were linear (r{sup 2} > 0.998) over the concentration range from 0.02 to 1 mg L{sup −1}. The recoveries of the eight analytes ranged

  6. A stimuli-responsive fluorescence platform for simultaneous determination of D-isoascorbic acid and Tartaric acid based on Maillard reaction product

    Science.gov (United States)

    Zhao, Yanmei; Yuan, Haiyan; Zhang, Xinling; Yang, Jidong

    2018-05-01

    An activatable fluorescence monitoring platform based on a novel Maillard reaction product from D-glucose and L-arginine was prepared through a facile one-pot approach and applied for simultaneous detection of D-isoascorbic acid and tartaric acid. In this work, the new Maillard reaction product GLA was first obtained, and its fluorescence intensity can be effectively quenched by KMnO4, resulting from a new complex (GLA-KMnO4) formation between GLA and KMnO4. Upon addition of D-isoascorbic acid or tartaric acid, an enhanced fluorescence was observed under the optimumed experimental conditions, indicating a stimuli-responsive fluorescence turn on platform for D-isoascorbic acid or tartaric acid can be developed. The corresponding experimental results showed that this turn on fluorescence sensing platform has a high sensitivity for D-isoascorbic acid or tartaric acid, because the detection limits were 5.9 μM and 21.5 μM, respectively. Additionally, this proposed sensing platform was applied to simultaneously detection of D-isoascorbic acid and tartaric acid in real tap water samples with satisfactory results.

  7. Ultra-performance liquid chromatography tandem mass-spectrometry (uplc-ms/ms) for the rapid, simultaneous analysis of thiamin, riboflavin, flavin adenine dinucleotide, nicotinamide and pyridoxal in human milk

    Science.gov (United States)

    A novel, rapid and sensitive Ultra Performance Liquid-Chromatography tandem Mass-Spectrometry (UPLC-MS/MS) method for the simultaneous determination of several B-vitamins in human milk was developed. Resolution by retention time or multiple reaction monitoring (MRM) for thiamin, riboflavin, flavin a...

  8. Simultaneous determination of dysprosium, holmium and erbium in high purity rare earth oxides by second order derivative spectrophotometry

    International Nuclear Information System (INIS)

    Anbu, M.; Prasada Rao, T.; Iyer, C. S. P.; Damodaran, A. D.

    1996-01-01

    High purity individual rare earth oxides are increasingly used as major components in lasers (Y 2 O 3 ), phosphors (YVO 3 , Eu 2 O 3 ), magnetic bubble memory films (Gd 2 O 3 ) and refractive-index lenses and fibre optics (La 2 O 3 ). The determination of individual lanthanides in high purity rare earth oxides is a more important and difficult task. This paper reports the utilization of higher order derivative spectrophotometry for the simultaneous determination of dysprosium, holmium and erbium in high purity rare earth oxides. The developed procedure is simple, reliable and allows the determination of 0.001 to 0.2% of dysprosium, holmium and erbium in several rare earth. (author). 9 refs, 2 figs, 2 tabs

  9. Simultaneous determination of borneol and its metabolite in rat plasma by GC–MS and its application to pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Xiu-Man Sun

    2014-10-01

    Full Text Available A gas chromatography mass spectrometry (GC–MS method has been developed and fully validated for the simultaneous determination of natural borneol (NB and its metabolite, camphor, in rat plasma. Following a single liquid–liquid extraction, the analytes were separated using an HP-5MS capillary column (0.25 mm×30 m×0.25 μm and analyzed by MS in the selected ion monitoring mode. Selected ion monitor (m/z of borneol, camphor and internal standard was 95, 95 and 128, respectively. Linearity, accuracy, precision and extraction recovery of the analytes were all satisfactory. The method was successfully applied to pharmacokinetic studies of NB after oral administration to Wistar rats. Keywords: Borneol, Camphor, Simultaneous determination, Pharmacokinetics, GC–MS

  10. Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben in Sucralfate Suspension Using High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Rajesh M. Kashid

    2011-01-01

    Full Text Available A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P. and propyl paraben (P.P. is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50 on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

  11. High performance liquid chromatography for simultaneous determination of xipamide, triamterene and hydrochlorothiazide in bulk drug samples and dosage forms.

    Science.gov (United States)

    Abd El-Hay, Soad S; Hashem, Hisham; Gouda, Ayman A

    2016-03-01

    A novel, simple and robust high-performance liquid chromatography (HPLC) method was developed and validated for simultaneous determination of xipamide (XIP), triamterene (TRI) and hydrochlorothiazide (HCT) in their bulk powders and dosage forms. Chromatographic separation was carried out in less than two minutes. The separation was performed on a RP C-18 stationary phase with an isocratic elution system consisting of 0.03 mol L(-1) orthophosphoric acid (pH 2.3) and acetonitrile (ACN) as the mobile phase in the ratio of 50:50, at 2.0 mL min(-1) flow rate at room temperature. Detection was performed at 220 nm. Validation was performed concerning system suitability, limits of detection and quantitation, accuracy, precision, linearity and robustness. Calibration curves were rectilinear over the range of 0.195-100 μg mL(-1) for all the drugs studied. Recovery values were 99.9, 99.6 and 99.0 % for XIP, TRI and HCT, respectively. The method was applied to simultaneous determination of the studied analytes in their pharmaceutical dosage forms.

  12. [Simultaneous determination of delta-9-tetrahydrocannabinol cannabidiol and cannabinol in edible oil using ultra performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Aizhi; Wang, Quanlin; Mo, Shijie

    2010-11-01

    A method for the simultaneous determination of delta-9-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in edible oil was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with methanol, purified by an LC-Alumina-N solid phase extraction cartridge, separated and detected by the UPLC-MS/MS. Quantitative analysis was corrected by an isotope internal standard method using delta-9-THC-D3 as internal standard. Average recoveries for the target compounds varied from 68.0% to 101.6% with the relative standard deviations ranging from 7.0% to 20.1% at three spiked levels. The limits of detection (LOD) of the method were from 0.06-0.17 microg/kg and the limits of quantification (LOQ) were in the range of 0.20-0.52 microg/kg. The results showed that the method is able to meet the requirements for the simultaneous determination of THC, CBD and CBN in edible oil.

  13. Rapid and Simultaneous Determination of Acetylsalicylic Acid, Paracetamol, and Their Degradation and Toxic Impurity Products by HPLC in Pharmaceutical Dosage Forms

    OpenAIRE

    AKAY, Cemal

    2008-01-01

    Aims: Determinations of drug impurity and drug degradation products are very important from both pharmacological and toxicological perspectives. Establishment of monitoring methods for impurities and degradation products during pharmaceutical development is necessary because of their potential toxicity. The aim of this study was to develop a rapid and simultaneous determination method for paracetamol and acetylsalicylic acid (ACA) and their degradation and toxic impurity products by high perf...

  14. Development and application of a validated stability-indicating HPLC method for simultaneous determination of granisetron hydrochloride, benzyl alcohol and their main degradation products in parenteral dosage forms.

    Science.gov (United States)

    Hewala, Ismail; El-Fatatre, Hamed; Emam, Ehab; Mubrouk, Mokhtar

    2010-06-30

    A simple, rapid and sensitive reversed phase high performance liquid chromatographic method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, benzyl alcohol, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron) and benzaldehyde (the main degradation product of benzyl alcohol) in granisetron injections. The separation was achieved on Hypersil BDS C8 (250 mm x 4.6 mm i.d., 5 microm particle diameter) column using a mobile phase consisted of acetonitrile:0.05 M KH(2)PO(4):triethylamine (22:100:0.15) adjusted to pH 4.8. The column was maintained at 25 degrees C and 20 microL of solutions was injected. Photodiode array detector was used to test the peak purity and the chromatograms were extracted at 210 nm. Naphazoline hydrochloride was used as internal standard. The method was validated with respect to specificity, linearity, accuracy, precision, limit of quantitation and limit of detection. The validation acceptance criteria were met in all cases. Identification of the pure peaks was carried out using library match programmer and wavelengths of derivative optima of the spectrograms of the peaks. The method was successfully applied to the determination of the investigated drugs and their degradation products in different batches of granisetron injections. The method was proved to be sensitive for the determination down to 0.03 and 0.01% of granisetron degradation product and benzaldehyde, respectively, which are far below the compendia limits for testing these degradation products in their corresponding intact drugs. Copyright 2010 Elsevier B.V. All rights reserved.

  15. Hybrid MEFPI/FBG sensor for simultaneous measurement of strain and magnetic field

    Science.gov (United States)

    Chen, Mao-qing; Zhao, Yong; Lv, Ri-qing; Xia, Feng

    2017-12-01

    A hybrid fiber-optic sensor consisting of a micro extrinsic Fabry-Perot Interferometer (MEFPI) and an etched fiber Bragg grating (FBG) is proposed, which can measure strain and magnetic field simultaneously. The etched FBG is sealed in a capillary with ferrofluids to detect the surrounding magnetic field. FBG with small diameter will be more sensitive to magnetic field is confirmed by simulation results. The MEFPI sensor that is prepared through welding a short section of hollow-core fiber (HCF) with single-mode fiber (SMF) is effective for strain detection. The experiment shows that strain and magnetic field can be successfully simultaneously detected based on hybrid MEFPI/FBG sensor. The sensitivities of the strain and magnetic field intensity are measured to be up to 1.41 pm/με and 5.11 pm/mT respectively. There is a negligible effect on each other, hence simultaneously measuring strain and magnetic field is feasible. It is anticipated that such easy preparation, compact and low-cost fiber-optic sensors for simultaneous measurement of strain and magnetic field could find important applications in practice.

  16. First liquid chromatography method for the simultaneous determination of levofloxacin, pazufloxacin, gatifloxacin, moxifloxacin and trovafloxacin in human plasma.

    Science.gov (United States)

    Sousa, Joana; Alves, Gilberto; Campos, Gonçalo; Fortuna, Ana; Falcão, Amílcar

    2013-07-01

    For the first time a simple, selective and sensitive liquid chromatography method was developed and validated for the simultaneous determination of levofloxacin (LEV), pazufloxacin (PAZ), gatifloxacin (GAT), moxifloxacin (MOX) and trovafloxacin (TRO) in human plasma. Samples were pre-treated with acetonitrile for precipitation of plasma proteins followed by evaporation and reconstitution steps. Chromatographic separation of the analytes and norfloxacin, used as internal standard (IS), was performed under gradient elution on a LiChroCART(®) Purospher Star C18 column (55mm×4mm, 3μm). The mobile phase comprised a mixture of 0.1% aqueous formic acid adjusted to pH 3.0 with triethylamine, acetonitrile and methanol pumped at a flow rate of 1.0mL/min. The detector was set at excitation/emission wavelengths of 260/455nm. Calibration curves were linear (r(2)≥0.9923) in the ranges of 0.005-5μg/mL for GAT, 0.02-5μg/mL for LEV, PAZ and MOX and 0.04-5μg/mL for TRO. The intra and interday precision did not exceed 7.32% and the intra and interday accuracy ranged from -11.73 to 8.92%. The limits of quantification were established at 0.005μg/mL for GAT, 0.02μg/mL for LEV, PAZ and MOX and 0.04μg/mL for TRO. No endogenous or tested exogenous compounds were found to interfere at the retention times of the analytes and IS. Since the proposed method proved to be reliable for the quantitative determination of LEV, PAZ, GAT, MOX and TRO it may be a useful tool for routine analysis and to support clinical pharmacokinetic and toxicological studies involving these antibiotics. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Highly sensitive luminescence method of scandium determination in the products of metallurgical reprocessing

    International Nuclear Information System (INIS)

    Matveets, M.A.; Akhmetova, S.D.

    1988-01-01

    Highly sensitive reaction of scandium with 1,10-phenanthroline and eosin is used for the development of luminescence method of its determination in metallurgical products. The effect of interfering elements is eliminated by scandium extraction with monocarboxylic acids. The method permits to determine scandium content from 5 x 10 -5 % (Sr 0.15 - 0.25)

  18. A procedure for the improvement in the determination of a TXRF spectrometer sensitivity curve

    International Nuclear Information System (INIS)

    Bennun, Leonardo; Sanhueza, Vilma

    2010-01-01

    A simple procedure is proposed to determine the total reflection X-ray fluorescence (TXRF) spectrometer sensitivity curve; this procedure provides better accuracy and exactitude than the standard established method. It uses individual pure substances instead of the use of vendor-certified values of reference calibration standards, which are expensive and lack any method to check their quality. This method avoids problems like uncertainties in the determination of the sensitivity curve according to different standards. It also avoids the need for validation studies between different techniques, in order to assure the quality of their TXRF results. (author)

  19. Highly sensitive interference-free electrochemical determination of pyridoxine at graphene modified electrode: Importance in Parkinson and Asthma treatments.

    Science.gov (United States)

    Raj, M Amal; Gowthaman, N S K; John, S Abraham

    2016-07-15

    To reduce the side effects in the medication of Parkinson and Asthma, pyridoxine (PY) is administered along with l-3,4-dihydroxyphenyl alanine (l-dopa) and theophylline (TP), respectively. However, excessive dosage of PY leads to nervous disorder. Thus, a sensitive and selective electrochemical method was developed for the determination of PY in the presence of major interferences including TP, l-dopa, ascorbic acid (AA) and riboflavin (RB) using electrochemically reduced graphene oxide (ERGO) film modified glassy carbon electrode (GCE) in this paper. The ERGO fabrication process involves the nucleophilic substitution of graphene oxide at basic pH on amine terminal of 1,6-hexadiamine which was pre-assembled on GCE followed by electrochemical reduction. The electrocatalytic activity of the ERGO modified electrode was examined towards the oxidation of PY. It greatly enhanced the oxidation current of PY in contrast to bare and GO modified GCEs due to facile electron transfer besides π-π interaction between ERGO film and PY. Since TP and l-dopa drugs antagonize the drug action of PY, ERGO modified GCE was also used for the simultaneous determination of PY and l-dopa and PY and TP. Further, the selective determination of PY in the presence of other water soluble vitamins such as ascorbic acid and riboflavin was also demonstrated. Using amperometry, detection of 100nM PY was achieved and the detection limit was found to be 5.6×10(-8)M (S/N=3). The practical application of the present method was demonstrated by determining the concentration of PY in human blood serum and commercial drugs. Copyright © 2016 Elsevier Inc. All rights reserved.

  20. Simultaneous determination of aerosol optical thickness and water-leaving radiance from multispectral measurements in coastal waters

    Science.gov (United States)

    Shi, Chong; Nakajima, Teruyuki

    2018-03-01

    Retrieval of aerosol optical properties and water-leaving radiance over ocean is challenging since the latter mostly accounts for ˜ 10 % of the satellite-observed signal and can be easily influenced by the atmospheric scattering. Such an effort would be more difficult in turbid coastal waters due to the existence of optically complex oceanic substances or high aerosol loading. In an effort to solve such problems, we present an optimization approach for the simultaneous determination of aerosol optical thickness (AOT) and normalized water-leaving radiance (nLw) from multispectral satellite measurements. In this algorithm, a coupled atmosphere-ocean radiative transfer model combined with a comprehensive bio-optical oceanic module is used to jointly simulate the satellite-observed reflectance at the top of atmosphere and water-leaving radiance just above the ocean surface. Then, an optimal estimation method is adopted to retrieve AOT and nLw iteratively. The algorithm is validated using Aerosol Robotic Network - Ocean Color (AERONET-OC) products selected from eight OC sites distributed over different waters, consisting of observations that covered glint and non-glint conditions from the Moderate Resolution Imaging Spectroradiometer (MODIS) instrument. Results show a good consistency between retrieved and in situ measurements at each site. It is demonstrated that more accurate AOTs are determined based on the simultaneous retrieval method, particularly in shorter wavelengths and sunglint conditions, where the averaged percentage difference (APD) of retrieved AOT is generally reduced by approximate 10 % in visible bands compared with those derived from the standard atmospheric correction (AC) scheme, since all the spectral measurements can be used jointly to increase the information content in the inversion of AOT, and the wind speed is also simultaneously retrieved to compensate the specular reflectance error estimated from the rough ocean surface model. For the

  1. Clinical introduction of simultaneous radiohyperthermotherapy

    International Nuclear Information System (INIS)

    Kuroda, Masahiro; Asaumi, Junichi; Hiraki, Yoshio; Inamura, Keiji; Tahara, Seiji; Mimura, Seiichi; Mikami, Yasutaka; Kawasaki, Shoji.

    1992-01-01

    Simultaneous radiohyperthermotherapy (SRH) is a combined hyperthermia-radiation therapy in which radiation is given during heating. Mutual interference between the high energy radiotherapy system (Toshiba LMR-15A) and the 13.56 MHz capacitive heating system (Omron HEH-500C) was examined using phantoms prior to clinical trials. Phantoms were irradiated and heated simultaneously at right angles. The energy and flatness of irradiation were measured using films and were not affected by the heating system within the range of clinical use. The temperature increase was measured with a thermocouple thermometer, and the temperature distribution was determined by liquid crystal thermometer. The high energy radiotherapy system did not affect the heating device set power, the temperature increase and distribution during simultaneous treatment. This study clarified that these apparatuses work simultaneously without clinically significant mutual interference. SRH using these apparatuses can be safely applied to clinical study. (author)

  2. Epicutaneous aeroallergen sensitization in atopic dermatitis infants - determining the role of epidermal barrier impairment.

    Science.gov (United States)

    Boralevi, F; Hubiche, T; Léauté-Labrèze, C; Saubusse, E; Fayon, M; Roul, S; Maurice-Tison, S; Taïeb, A

    2008-02-01

    Sensitization to atopens is an early phenomenon that overlaps with the onset of atopic dermatitis (AD) in infancy. Early epidermal barrier impairment may facilitate the epicutaneous penetration of atopens. To correlate transepidermal water loss (TEWL) and aeroallergen sensitization in infants with AD. In this cross-sectional study we enrolled 59 AD children and 30 controls aged 3-12 months. Transepidermal water loss in uninvolved skin, specific immunoglobulin E, atopy patch test (APT) and skin prick tests were performed with respect to seven aeroallergens, i.e., Dermatophagoides pteronyssinus, D. farinae, cat, dog, birch pollen, ambrosia, and cockroach. Environmental conditions were assessed by a questionnaire, and the house dust mite (HDM) concentration was determined in dust samples. Eighty-nine percent of AD infants had a positive APT vs one out of eleven controls. AD infants had a significantly higher mean TEWL than controls (27.4 vs 11.1 g/m(2)/h, P cats, and dogs at home. This study confirms the high prevalence of delayed sensitization to indoor and outdoor aeroallergens in AD infants, and shows that the higher the TEWL, the higher the prevalence of sensitization to aeroallergens. These data are in favor of a major role of a constitutive epidermal barrier impairment in determining early atopen sensitization in infants with AD.

  3. Simultaneous quantitative determination of eight index constituents and compatibility changes in Longchai Decoction by UPLC–Q-TOF-MS

    Directory of Open Access Journals (Sweden)

    Yizhi Zhou

    2013-07-01

    Full Text Available The goal of this research was to develop a simple, rapid and sensitive method for simultaneous quantitative determination of salidroside, gardenoside, liquiritin, baicalin, wogonoside, wogonin, saikosaponin A and saikosaponin D in Longchai Decoction by ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC–Q-TOF-MS, in order to control the quality of Longchai Decoction and to analyze the changes of chemical components before and after the compatibility of the component herb drugs. The chromatographic separation was performed on the Waters ACQUITY BEH C18 column (2.1 mm×100 mm, 1.8 μm using the mixture of acetonitrile and 0.1% (v/v methanoic acid as mobile phase with a gradient elution program at the flow rate of 0.3 mL/min and the column temperature of 30 °C. The eight components of the standards achieved baseline separation. Regression analysis revealed a linear relationship (r2>0.9998 between the contents and the peak areas of the mixed standard substances. The average recovery rates were between 99.72% and 102.13% with RSD values were less than 2.82% (n=5. The obtained results indicated that the content of index components were higher in co-decoction compared to mixed decoction. This method with a good resolution and high precision can be used for the quality control of Longchai Decoction.

  4. Simultaneous determination of acidic 3,4-dihydroxyphenylalanine metabolites and 5-hydroxyindole-3-acetic acid in urine by high-performance liquid chromatography

    NARCIS (Netherlands)

    Stroomer, A. E.; Overmars, H.; Abeling, N. G.; van Gennip, A. H.

    1990-01-01

    We describe a simple and rapid quantitative method for the simultaneous determination of 3,4-dihydroxyphenylalanine acid metabolites and 5-hydroxyindole-3-acetic acid. After solvent extraction from acidified urine, the acids are analyzed by reversed-phase high-performance liquid chromatography. For

  5. Simultaneous determination of moxifloxacin and ofloxacin in physiological fluids using high performance liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Khan, Fahim Ullah; Nasir, Fazli; Iqbal, Zafar; Khan, Ismail; Shahbaz, Naila; Hassan, Muhammad; Ullah, Farhad

    2016-04-01

    A novel, sensitive and validated RP-HPLC-UV method was developed for simultaneous determination of moxifloxacin and ofloxacin using timolol maleate as internal standard in physiological fluids. Different experimental parameters were optimized and validated according to international guidelines. Complete separation of the analytes was achieved with Kromasil 100-5C18 analytical column (250mm×4.6mm×5μm), methanol and 0.05% trifloroacetic acid (TFA) (38:62v/v) were used as mobile phase, pumped at flow rate of 1.1ml/min in isocratic phase, column oven temperature maintained at 45°C and detection wavelength of 290nm. Protein precipitation method was applied to extract the drugs from human plasma and bovine aqueous humor samples using methanol as precipitating solvent. This method is linear in concentration range of 0.018-100μg/ml for moxifloxacin and 0.014-20μg/ml for ofloxacin. The recoveries of the method were 97.52 and 97.39% in human plasma for MX and OFN respectively, while in aqueous humor 94.48% for MX. The LOD values in plasma were found to be 10.0 and 8.00ng/ml for MX and OFN respectively, while their respective LOQ values were 18.0 and 14ng/ml. In aqueous humor the LOD and LOQ for MX were 16.0 and 24ng/ml respectively. In future, this method will be used to study the pharmacokinetic profile of moxifloxacin and ofloxacin in biological fluids and pharmaceutical products. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. [Simultaneous determination of eight kinds of conjunct bile acids in human bile by R-HPLC].

    Science.gov (United States)

    Dai, Z; Tan, G; Qian, K; Chen, X

    1997-01-01

    A method for the simultaneous determination of eight kinds of conjunct bile acids in human bile was developed by HPLC. They were separated on a YWG-C18 (3 microns) column at 30 degrees C, with methanol/water (65/35, V/V, pH3.0) as mobile phase, and detection wavelength at UV 210 nm. The linear ranges were 50-1,000 microns.ml-1, the recoveries were 91.2%-108.6%. The biles of 30 cases with cholelithiasis cholecystolithiasis and 20 cases without gallstone were detected by HPLC. The results showed that the constitution of bile acids was different between patients with cholelithiasis cholecystolithiasis and patients without gallstone.

  7. Development and application of a validated stability-indicating high-performance liquid chromatographic method using photodiode array detection for simultaneous determination of granisetron, methylparaben, propylparaben, sodium benzoate, and their main degradation products in oral pharmaceutical preparations.

    Science.gov (United States)

    Hewala, Ismail; El-Fatatry, Hamed; Emam, Ehab; Mabrouk, Mokhtar

    2011-01-01

    A simple, rapid, and sensitive RP-HPLC method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron), sodium benzoate, methylparaben, propylparaben, and 4-hydroxybenzoic acid (the main degradation product of parabens) in granisetron oral drops and solutions. The separation of the compounds was achieved within 8 min on a SymmetryShield RP18 column (100 x 4.6 mm id, 3.5 microm particle size) using the mobile phase acetonitrile--0.05 M KH2PO4 buffered to pH 3 using H3PO4 (3+7, v/v). The photodiode array detector was used to test the purity of the peaks, and the chromatograms were extracted at 240 nm. The method was validated, and validation acceptance criteria were met in all cases. The robust method was successfully applied to the determination of granisetron and preservatives, as well as their degradation products in different batches of granisetron oral drops and solutions. The method proved to be sensitive for determination down to 0.04% (w/w) of granisetron degradation product relative to granisetron and 0.03% (w/w) 4-hydroxybenzoic acid relative to total parabens.

  8. An integrated scheme for the simultaneous determination of biogenic amines, precursor amino acids, and related metabolites by liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Oka, K; Kojima, K; Togari, A; Nagatsu, T; Kiss, B

    1984-06-08

    A new method using high-performance liquid chromatography with electrochemical detection (HPLC-ED) for the simultaneous determination of monoamines, their precursor amino acids, and related major metabolites in small samples of brain tissue weighing from 0.5 to 50 mg is described. The method is based on the preliminary isolation of monoamines (dopamine, norepinephrine, epinephrine, and serotonin), their precursor amino acids (tyrosine, 3,4-dihydroxyphenylalanine, tryptophan and 5-hydroxytryptophan), and their major metabolites (3-methoxytyramine, normetanephrine, 3,4-dihydroxyphenylacetic acid, homovanillic acid, vanillylmandelic acid, 3-methoxy-4-hydroxyphenylethyleneglycol, and 5-hydroxyindoleacetic acid) by chromatography on small columns of Amberlite CG-50 and Dowex 50W, and by ethyl acetate extraction. All the compounds in the four isolated fractions were measured by HPLC-ED on a reversed-phase column under four different conditions. The sensitivity was from 0.1 to 40 pmol, depending on the substances analysed. This newly established method was applied to the study of the effects of an aromatic L-amino acid decarboxylase inhibitor (NSD-1015) and a monoamine oxidase inhibitor (pargyline) on the levels of monoamines, their precursor amino acids and their major metabolites in brain regions of mice.

  9. Simultaneous Determination of Ibuprofen and Caffeine in Urine Samples by Combining MCR-ALS and Excitation-emission Data

    Directory of Open Access Journals (Sweden)

    Masoumeh Mohammadnejad

    2016-06-01

    Full Text Available Second order advantage of excitation-emission fluorescence matrix was applied for the simultaneous determination of ibuprofen and caffeine. The proposed method is based on the measurement of the native fluorescence and recording emission spectra of ibuprofen and caffeine in different excitation wavelengths. The mixture of these compounds was resolved by multivariate curve resolution coupled with alternative least squares (MCR-ALS on constructed matrix. The EEM spectra were recorded at excitation wavelengths from 250-275 nm; the emission wavelengths ranged from 275-400 nm. For each particular quantitative determination, an augmented matrix was defined. The resolution of each augmented-data matrix gave an estimation of the excitation and emission spectra of the species included in the model. Ibuprofen and caffeine were determined in concentration range from 0.10-8.00 and 0.50-15.00 mg ml-1, respectively. The minimal sample pretreatment and relatively low running cost, make this method a good alternative to existing methods for determination of the analytes in urine samples.

  10. Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine.

    Science.gov (United States)

    Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming

    2013-05-24

    We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant kb, were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0×10(-8) to 2.0×10(-5) mol L(-1), with a low limit of detection (LOD) of 1.25×10(-8) mol L(-1) for SY and 1.43×10(-8) mol L(-1) for TT (SN(-1)=3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant differences were found. By the treatment of the experimental data, the electrochemical reaction mechanisms of SY and TT both involved a one-electron-one-proton-transfer process. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Rapid and sensitive enzymatic-radiochemical assay for the determination of triglycerides

    International Nuclear Information System (INIS)

    Khoo, J.C.; Miller, E.; Goldberg, D.I.

    1987-01-01

    An enzymatic-radiochemical method suitable for the determination of triglyceride levels of cells in culture is described. The method is based on the enzymatic hydrolysis of triglycerides to free fatty acids which then complex with 63 Ni. The method is rapid, accurate, and inexpensive. The procedure extends the sensitivity of triglyceride measurement to as low as 0.25 nanomoles

  12. Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

    OpenAIRE

    M. Kashid, Rajesh; G. Singh, Santosh; Singh, Shrawan

    2011-01-01

    A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precisi...

  13. Determining Factors for Fast Corneal Sensitivity Recovery After Pterygium Excision

    OpenAIRE

    Julio Morán, Gemma; Campos, Pamela; Pujol Vives, Pere; Munguia, Aitana; Mas Aixalà, Enric

    2016-01-01

    Purpose: To establish determining factors for fast corneal sensitivity (CS) recovery after pterygium excision. Methods: Thirty-two eyes of 14 males and 18 females with primary nasal pterygium were recruited. Differences in CS (in the 4 quadrants and the center using a Cochet–Bonnet esthesiometer), pterygium corneal area (PCA), tear osmolarity, tear break-up time, Schirmer test, and ocular symptoms were analyzed before and 1 month after lesion excision. The relationship between CS recovery...

  14. Simultaneous determination of fumonisins B1, B2 and B3 contaminants in maize by ultra high-performance liquid chromatography tandem mass spectrometry

    International Nuclear Information System (INIS)

    Ren Yiping; Zhang Yu; Han Shiyun; Han Zheng; Wu Yongning

    2011-01-01

    The present work developed an analytical method for simultaneous determination of fumonisins B 1 , B 2 and B 3 residues in maize by ultra high-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UHPLC-MS/MS) under the multiple reaction monitoring (MRM) mode, and especially focused on the optimization of extraction, clean-up, UHPLC separation and MS/MS parameters. The method involves addition of fumonisins isotope internal standards, extraction with a mixture of acetonitrile and water and clean-up with solid-phase extraction (SPE) cartridges before UHPLC-MS/MS analysis. A single-laboratory method validation was conducted by testing three different spiking levels for repeatability and recovery according to International Union of Pure and Applied Chemistry (IUPAC) guidelines. The LOQ of FB 1 , FB 2 and FB 3 were 1.50, 1.65 and 0.4 μg kg -1 , respectively, which were lower than the criteria of EU, USA and other countries regarding minimum residue limits of fumonisins in foods including baby foods and feedstuffs. Recoveries of three fumonisins ranged from 80.9% to 97.0% with RSD values of 2.4-11.1%.The advantages of this method include simple pretreatment, rapid determination and high sensitivity, and it fulfills the requirements for food analysis with respect to minimum residue limits of fumonisins in various countries.

  15. Simultaneous determination of flurbiprofen and its hydroxy metabolite in human plasma by liquid chromatography-tandem mass spectrometry for clinical application.

    Science.gov (United States)

    Lee, Hye-In; Choi, Chang-Ik; Byeon, Ji-Yeong; Lee, Jung-Eun; Park, So-Young; Kim, Young-Hoon; Kim, Se-Hyung; Lee, Yun-Jeong; Jang, Choon-Gon; Lee, Seok-Yong

    2014-11-15

    Flurbiprofen (FLB) is one of the phenylalkanoic acid derivatives of non-steroidal anti-inflammatory drugs used for the management of pain and inflammation in patients with arthritis. We developed and validated a rapid and sensitive high-performance liquid chromatography analytical method utilizing tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of FLB and its major metabolite, 4'-hydroxyflurbiprofen (4'-OH-FLB), in human plasma. Probenecid was used as an internal standard (IS). After liquid-liquid extraction with methyl t-butyl ether, chromatographic separation of the two analytes was achieved using a reversed-phase Luna C18 column (2.0mm×50mm, 5μm particles) with a mobile phase of 10mM ammonium formate buffer (pH 3.5)-methanol (15:85, v/v) and quantified by MS/MS detection in ESI negative ion mode. The flow rate of the mobile phase was 250μl/min and the retention times of FLB, 4'-OH-FLB, and IS were 1.1, 0.8, and 0.9min, respectively. The calibration curves were linear over a range of 0.01-10μg/ml for FLB and 0.01-1μg/ml for 4'-OH-FLB. The lower limit of quantifications using 100μl of human plasma was 0.01μg/ml for both analytes. The mean accuracy and precision for intra- and inter-run validation of FLB and 4'-OH-FLB were all within acceptable limits. The present HPLC-MS/MS method showed improved sensitivity for quantification of the FLB and its major metabolite in human plasma compared with previously described analytical methods. The validated method was successfully applied to a pharmacokinetic study in humans. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. A review of analytical procedures for the simultaneous determination of medically important veterinary antibiotics in environmental water: Sample preparation, liquid chromatography, and mass spectrometry.

    Science.gov (United States)

    Kim, Chansik; Ryu, Hong-Duck; Chung, Eu Gene; Kim, Yongseok; Lee, Jae-Kwan

    2018-07-01

    Medically important (MI) antibiotics are defined by the United States Food and Drug Administration as drugs containing certain active antimicrobial ingredients that are used for the treatment of human diseases or enteric pathogens causing food-borne diseases. The presence of MI antibiotic residues in environmental water is a major concern for both aquatic ecosystems and public health, particularly because of their potential to contribute to the development of antimicrobial-resistant microorganisms. In this article, we present a review of global trends in the sales of veterinary MI antibiotics and the analytical methodologies used for the simultaneous determination of antibiotic residues in environmental water. According to recently published government reports, sales volumes have increased steadily, despite many countries having adopted strategies for reducing the consumption of antibiotics. Global attention needs to be directed urgently at establishing new management strategies for reducing the use of MI antimicrobial products in the livestock industry. The development of standardized analytical methods for the detection of multiple residues is required to monitor and understand the fate of antibiotics in the environment. Simultaneous analyses of antibiotics have mostly been conducted using high-performance liquid chromatography-tandem mass spectrometry with a solid-phase extraction (SPE) pretreatment step. Currently, on-line SPE protocols are used for the rapid and sensitive detection of antibiotics in water samples. On-line detection protocols must be established for the monitoring and screening of unknown metabolites and transformation products of antibiotics in environmental water. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. RIA Quick, AUSRIA II-125, AUSAB. Comparative study on isolated and simultaneous radioimmunoassay of hepatitis B surface antigen and antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Kselikova, M; Urbankova, J [Institut fuer Haematologie und Bluttransfusion, Prag (Czechoslovakia)

    1983-01-01

    The surface antigen of hepatitis B (HBsAg) and the antibodies against HBsAg can be determined separately by the radioimmunoassay (RIA) test kits AUSRIA II-125 and AUSAB, respectively. Using the test kit RIA Quick (IMMUNO, Wien) it is possible to perform both the determinations in one preparation simultaneously. The sensitivity of RIA Quick for HBsAg corresponds to that of AUSRIA II-125 and for HBsAB it is considerably lower than that of AUSAB. RIA Quick is of excellent technical design and is by a quarter cheaper than the kits for isolated determination of HBsAg and HBsAb.

  18. Multiresponse optimization of a UPLC method for the simultaneous determination of tryptophan and 15 tryptophan-derived compounds using a Box-Behnken design with a desirability function.

    Science.gov (United States)

    Setyaningsih, Widiastuti; Saputro, Irfan E; Carrera, Ceferino A; Palma, Miguel; Barroso, Carmelo G

    2017-06-15

    A Box-Behnken design was used in conjunction with multiresponse optimization based on the desirability function to carry out the simultaneous separation of tryptophan and 15 derivatives by Ultra Performance Liquid Chromatography. The gradient composition of the mobile phase and the flow rate were optimized with respect to the resolution of severely overlapping chromatographic peaks and the total run time. Two different stationary phases were evaluated (hybrid silica and a solid-core-based C 18 column). The methods were validated and a suitable sensitivity was found for all compounds in the concentration range 1-100μgL -1 (R 2 >0.999). High levels of repeatability and intermediate precision (CV less than 0.25% and 1.7% on average for the retention time and the signal area, respectively) were obtained. The new method was applied to the determination tryptophan and its derivatives in black pigmented glutinous and non-glutinous rice grain samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Simultaneous determination of paracetamol, 4-Aminophenol, 4-Chloroacetanilid, Benzyl alcohol,Benzaldehyde and EDTA by HPLC methodin paracetamol injection ampoule

    Directory of Open Access Journals (Sweden)

    Ali Merrikhi Khosroshahi

    2016-06-01

    Full Text Available Paracetamol that is known as acetaminophen have the most consume as an analgesic and antipyretic drug in the world. That is formulated in single compound or mixture at many forms such as tablets, syrups, suspensions and drops. The last form is intravenous injections. Paracetamol derived from 4-minophenol which is synthesized by acylated the P-acetaminophenol and acetic anhydride. 4-aminophenol is the main impurity at manufacturing of paracetamol which could produce by hydrolysis during storage or synthesis under normal conditions (temperature, pH, etc.. Also, 4-chloroacetanilid may be observed as an impurity in the raw material of paracetamol synthesis. Benzyl alcohol is a preservative that used in Paracetamol for injection. It will be very important if there are analytical techniques to measuring paracetamol and its degradation products accurately and easily. Undoubtedly the most important and widely used, separation technique is chromatography. There are several reports about separation and quantitative determination of paracetamol lonely or simultaneous determination of paracetamol and 4-aminophenol. In this paper investigated simultaneous determination of paracetamol, 4-aminophenol, 4-chloroacetanilid, benzyl alcohol, benzaldehyde, and EDTA in paracetamol for injection ampoules by high performance liquid chromatography. By changing the ratio of mixing methanol and acetonitrile as mobile phase at the wavelength of 215 nm and pH=3 separation of all compounds were completely done.

  20. Simultaneous in situ derivatization and ultrasound-assisted dispersive magnetic solid phase extraction for thiamine determination by spectrofluorimetry.

    Science.gov (United States)

    Tarigh, Ghazale Daneshvar; Shemirani, Farzaneh

    2014-06-01

    A simple and rapid method for the simultaneous in situ derivatizaion, preconcentration and extraction of thiamine (vitamin B1) as a model analyte was developed by a novel quantitative method, namely ultrasound-assisted dispersive magnetic solid phase extraction spectrofluorimetry (USA-DMSPE-FL) from different real samples. This method consists of sample preparation, in situ derivatization, exhaustive extraction and clean up by a single process. High extraction efficiency and in situ derivatization in a short period of time is the main advantages of this procedure. For this purpose, the reusable magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was used as an adsorbent for preconcentration and determination of thiamine. Thiamine was, simultaneously, in situ derivatized as thiochrome by potassium hexacyanoferrate (III) and adsorbed on MMWCNT in an ultrasonic water bath. The MMWCNTs were then collected using an external magnetic field. Subsequently, the extracted thiochrome was washed from the surface of the adsorbent and determined by spectrofluorimetry. The developed method, which has been analytically characterized under its optimal operating conditions, allows the detection of the analyte in the samples with method detection limits of 0.37 µg L(-1). The repeatability of the method, expressed as the relative standard deviation (RSD, n=6), varies between 2.0% and 4.8% in different real samples, while the enhancement factor is 197. The proposed procedure has been applied for the determination of thiamine in biological (serum and urine), pharmaceutical (multivitamin tablet and B complex syrup) and foodstuff samples (cereal, wheat flour, banana and honey) with the good recoveries in the range from 90% to 105%. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. A dual enzymatic-biosensor for simultaneous determination of glucose and cholesterol in serum and peritoneal macrophages of diabetic mice: Evaluation of the diabetes-accelerated atherosclerosis risk

    Energy Technology Data Exchange (ETDEWEB)

    Huang Qilin; An Yarui; Tang Linlin; Jiang Xiaoli; Chen Hua; Bi Wenji [Department of Chemistry, East China Normal University, Shanghai 200062 (China); Wang Zhongchuan [Department of Anorectal Surgery, Xinhua Hospital, Affiliated to School of Medicine of Shanghai Jiaotong University, Shanghai 200092 (China); Zhang Wen, E-mail: wzhang@chem.ecnu.edu.cn [Department of Chemistry, East China Normal University, Shanghai 200062 (China)

    2011-11-30

    Graphical abstract: In this paper, we reported a novel dual enzymatic-biosensor for simultaneous determination of glucose and cholesterol in serum and peritoneal macrophages (PMs) of diabetic mice to evaluate the diabetes-accelerated atherosclerosis risk. The biosensor was firstly modified with a poly-thionine (PTH) film as electron transfer mediator (ETM), then the gold nanoparticles (GNPs) were covered on the surface of PTH to act as tiny conduction centers for facilitating the electron transfer between enzymes and electrode. The schematic of the dual biosensor is shown in figure. The developed dual biosensor had good electrocatalytic activity toward the oxidations of glucose and cholesterol, exhibited a linear range from 0.008 mM to 6.0 mM for glucose with a detection limit of 2.0 {mu}M, and a linear range from 0.002 mM to 1.0 mM for cholesterol with a detection limit of 0.6 {mu}M. The results of the diabetic mice demonstrated that the cholesterol level was not changed obviously with the increase of glucose level in serum, while the cholesterol level was enhanced together with the increase of the glucose level in PMs. Previous studies have shown that the large accumulation of cholesterol in macrophage could lead to macrophage foam cell formation, the hallmark of early atherosclerosis. These findings indicated the possibility that high glucose induced by diabetes might increase the macrophage cholesterol level to further accelerate atherosclerosis development. Highlights: Black-Right-Pointing-Pointer A novel biosensor was developed to determine glucose and cholesterol simultaneously. Black-Right-Pointing-Pointer The dual enzymatic-biosensor has good selectivity and high sensitivity. Black-Right-Pointing-Pointer We determined glucose and cholesterol in the real samples of diabetic mice. Black-Right-Pointing-Pointer The results showed that high glucose might increase the macrophage cholesterol level. Black-Right-Pointing-Pointer It provided useful experimental

  2. A dual enzymatic-biosensor for simultaneous determination of glucose and cholesterol in serum and peritoneal macrophages of diabetic mice: Evaluation of the diabetes-accelerated atherosclerosis risk

    International Nuclear Information System (INIS)

    Huang Qilin; An Yarui; Tang Linlin; Jiang Xiaoli; Chen Hua; Bi Wenji; Wang Zhongchuan; Zhang Wen

    2011-01-01

    Graphical abstract: In this paper, we reported a novel dual enzymatic-biosensor for simultaneous determination of glucose and cholesterol in serum and peritoneal macrophages (PMs) of diabetic mice to evaluate the diabetes-accelerated atherosclerosis risk. The biosensor was firstly modified with a poly-thionine (PTH) film as electron transfer mediator (ETM), then the gold nanoparticles (GNPs) were covered on the surface of PTH to act as tiny conduction centers for facilitating the electron transfer between enzymes and electrode. The schematic of the dual biosensor is shown in figure. The developed dual biosensor had good electrocatalytic activity toward the oxidations of glucose and cholesterol, exhibited a linear range from 0.008 mM to 6.0 mM for glucose with a detection limit of 2.0 μM, and a linear range from 0.002 mM to 1.0 mM for cholesterol with a detection limit of 0.6 μM. The results of the diabetic mice demonstrated that the cholesterol level was not changed obviously with the increase of glucose level in serum, while the cholesterol level was enhanced together with the increase of the glucose level in PMs. Previous studies have shown that the large accumulation of cholesterol in macrophage could lead to macrophage foam cell formation, the hallmark of early atherosclerosis. These findings indicated the possibility that high glucose induced by diabetes might increase the macrophage cholesterol level to further accelerate atherosclerosis development. Highlights: ► A novel biosensor was developed to determine glucose and cholesterol simultaneously. ► The dual enzymatic-biosensor has good selectivity and high sensitivity. ► We determined glucose and cholesterol in the real samples of diabetic mice. ► The results showed that high glucose might increase the macrophage cholesterol level. ► It provided useful experimental evidences for diabetes-accelerate atherosclerosis. - Abstract: In this paper, a novel dual enzymatic-biosensor is described for

  3. Rapid and simultaneous determination of neptunium and plutonium isotopes in environmental samples by extraction chromatography using sequential injection analysis and ICP-MS

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2010-01-01

    plutonium and neptunium in three reference materials were in agreement with the recommended or literature values at the 0.05 significance level. The developed method is suitable for the analysis of up to 10 g of soil and 20 g of seaweed samples. The extraction chromatographic separation within the SI system......This paper reports an automated analytical method for rapid and simultaneous determination of plutonium isotopes (239Pu and 240Pu) and neptunium (237Np) in environmental samples. An extraction chromatographic column packed with TrisKem TEVA® resin was incorporated in a sequential injection (SI...... for a single sample takes less than 1.5 h. As compared to batchwise procedures, the developed method significantly improves the analysis efficiency, reduces the labor intensity and expedites the simultaneous determination of plutonium and neptunium as demanded in emergency actions....

  4. Chemical reactivation of resin-embedded pHuji adds red for simultaneous two-color imaging with EGFP

    Science.gov (United States)

    Guo, Wenyan; Liu, Xiuli; Liu, Yurong; Gang, Yadong; He, Xiaobin; Jia, Yao; Yin, Fangfang; Li, Pei; Huang, Fei; Zhou, Hongfu; Wang, Xiaojun; Gong, Hui; Luo, Qingming; Xu, Fuqiang; Zeng, Shaoqun

    2017-01-01

    The pH-sensitive fluorescent proteins enabling chemical reactivation in resin are useful tools for fluorescence microimaging. EGFP or EYFP is good for such applications. For simultaneous two-color imaging, a suitable red fluorescent protein is an urgent need. Here a pH-sensitive red fluorescent protein, pHuji, is selected and verified to remain pH-sensitive in HM20 resin. We observe 183% fluorescence intensity of pHuji in resin-embeded mouse brain and 29.08-fold fluorescence intensity of reactivated pHuji compared to the quenched state. pHuji and EGFP can be quenched and chemically reactivated simultaneously in resin, thus enabling simultaneous two-color micro-optical sectioning tomography of resin-embedded mouse brain. This method may greatly facilitate the visualization of neuronal morphology and neural circuits to promote understanding of the structure and function of the brain. PMID:28717566

  5. Simultaneous determination of linagliptin and metformin by reverse phase-high performance liquid chromatography method: An application in quantitative analysis of pharmaceutical dosage forms

    Directory of Open Access Journals (Sweden)

    Prathyusha Vemula

    2015-01-01

    Full Text Available To enhance patient compliance toward treatment in diseases like diabetes, usually a combination of drugs is prescribed. Therefore, an anti-diabetic fixed-dose combination of 2.5 mg of linagliptin 500 mg of metformin was taken for simultaneous estimation of both the drugs by reverse phase-high performance liquid chromatography (RP-HPLC method. The present study aimed to develop a simple and sensitive RP-HPLC method for the simultaneous determination of linagliptin and metformin in pharmaceutical dosage forms. The chromatographic separation was designed and evaluated by using linagliptin and metformin working standard and sample solutions in the linearity range. Chromatographic separation was performed on a C 18 column using a mobile phase of 70:30 (v/v mixture of methanol and 0.05 M potassium dihydrogen orthophosphate (pH adjusted to 4.6 with orthophosphoric acid delivered at a flow rate of 0.6 mL/min and UV detection at 267 nm. Linagliptin and metformin shown linearity in the range of 2-12 μg/mL and 400-2400 μg/mL respectively with correlation co-efficient of 0.9996 and 0.9989. The resultant findings analyzed for standard deviation (SD and relative standard deviation to validate the developed method. The retention time of linagliptin and metformin was found to be 6.3 and 4.6 min and separation was complete in <10 min. The method was validated for linearity, accuracy and precision were found to be acceptable over the linearity range of the linagliptin and metformin. The method was found suitable for the routine quantitative analysis of linagliptin and metformin in pharmaceutical dosage forms.

  6. Position-Sensitive Detector with Depth-of-Interaction Determination for Small Animal PET

    CERN Document Server

    Fedorov, A; Kholmetsky, A L; Korzhik, M V; Lecoq, P; Lobko, A S; Missevitch, O V; Tkatchev, A

    2002-01-01

    Crystal arrays made of LSO and LuAP crystals 2x2x10 mm pixels were manufactured for evaluation of detector with depth-of-interaction (DOI) determination capability intended for small animal positron emission tomograph. Position-sensitive LSO/LuAP phoswich DOI detector based on crystal 8x8 arrays and HAMAMATSU R5900-00-M64 position-sensitive multi-anode photomultiplier tube was developed and evaluated. Time resolution was found to be not worse than 1.0 ns FWHM for both layers, and spatial resolution mean value was 1.5 mm FWHM for the center of field-of-view.

  7. A device for simultaneous spin analysis of ultracold neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Afach, S. [Institute for Particle Physics, ETH Zuerich, Zuerich (Switzerland); Paul Scherrer Institute, Villigen-PSI (Switzerland); Jena University Hospital, Hans Berger Department of Neurology, Jena (Germany); Ban, G.; Lefort, T.; Lemiere, Y.; Naviliat-Cuncic, O.; Quemener, G. [Universite de Caen, CNRS/IN2P3, LPC Caen ENSICAEN, Caen (France); Bison, G.; Chowdhuri, Z.; Daum, M.; Henneck, R.; Lauss, B.; Mtchedlishvili, A.; Schmidt-Wellenburg, P.; Zsigmond, G. [Paul Scherrer Institute, Villigen-PSI (Switzerland); Bodek, K.; Rawlik, M.; Rozpedzik, D.; Zejma, J. [Jagiellonian University, Marian Smoluchowski Institute of Physics, Cracow (Poland); Fertl, M.; Franke, B.; Kirch, K.; Komposch, S. [Institute for Particle Physics, ETH Zuerich, Zuerich (Switzerland); Paul Scherrer Institute, Villigen-PSI (Switzerland); Geltenbort, P. [Institut Laue-Langevin, Grenoble (France); Grujic, Z.D.; Kasprzak, M.; Weis, A. [University of Fribourg, Physics Department, Fribourg (Switzerland); Hayen, L.; Severijns, N.; Wursten, E. [Katholieke Universiteit Leuven, Instituut voor Kernen Stralingsfysica, Leuven (Belgium); Helaine, V. [Paul Scherrer Institute, Villigen-PSI (Switzerland); Universite de Caen, CNRS/IN2P3, LPC Caen ENSICAEN, Caen (France); Kermaidic, Y.; Pignol, G.; Rebreyend, D. [Universite Grenoble Alpes, CNRS/IN2P3, LPSC, Grenoble (France); Kozela, A. [Henryk Niedwodniczanski Institute for Nuclear Physics, Cracow (Poland); Krempel, J.; Piegsa, F.M. [Institute for Particle Physics, ETH Zuerich, Zuerich (Switzerland); Prashanth, P.N. [Paul Scherrer Institute, Villigen-PSI (Switzerland); Katholieke Universiteit Leuven, Instituut voor Kernen Stralingsfysica, Leuven (Belgium); Ries, D. [Paul Scherrer Institute, Villigen-PSI (Switzerland); Jena University Hospital, Hans Berger Department of Neurology, Jena (Germany); Roccia, S. [Universite Paris Sud, CNRS/IN2P3, CSNSM, Orsay campus (France); Wyszynski, G. [Institute for Particle Physics, ETH Zuerich, Zuerich (Switzerland); Jagiellonian University, Marian Smoluchowski Institute of Physics, Cracow (Poland)

    2015-11-15

    We report on the design and first tests of a device allowing for measurement of ultracold neutrons polarisation by means of the simultaneous analysis of the two spin components. The device was developed in the framework of the neutron electric dipole moment experiment at the Paul Scherrer Institute. Individual parts and the entire newly built system have been characterised with ultracold neutrons. The gain in statistical sensitivity obtained with the simultaneous spin analyser is (18.2 ± 6.1) % relative to the former sequential analyser under nominal running conditions. (orig.)

  8. Simultaneous spectrophotometric determination of trimethoprim and sulphamethoxazole following charge-transfer complexation with chloranilic acid

    Directory of Open Access Journals (Sweden)

    Olajire A. Adegoke

    2017-05-01

    Full Text Available A simple, accurate and precise simultaneous spectrophotometric method has been developed for the analysis of trimethoprim–sulphamethoxazole combination in pure and tablet dosage forms. The method involves direct charge transfer complexation of trimethoprim (TMP with chloranilic acid (CAA in acetonitrile–dioxane solvent mixture and complexation of sulphamethoxazole (SMZ after its hydrolysis in dilute H2SO4. Optimization of temperature and time revealed the superiority of room temperature and 20 and 30 min respectively for TMP and SMZ. Optimal detector responses were obtained at 520 and 440 nm and were therefore selected as working wavelength maxima for SMZ and TMP respectively. TMP and hydrolysed SMZ were combined with CAA at mole ratios of 1:1 and 1:3 respectively. Accuracies were generally less than 4% (estimated as degree of inaccuracy or error with a precision of the order of less than 2% on a three-day assessment. Physicochemical factors responsible for complex stability were estimated and related to the observed data. The method was successfully applied to the determination of TMP and SMZ in tablet dosage forms with accuracies comparable to the official BP method. There were no interferences from common tablet excipients and TMP complex did not interfere with the assay of SMZ. The developed method could find application in routine quality control of TMP–SMZ combination. It is the first reported full simultaneous colorimetric assay of TMP and SMZ using the same analytical reagent.

  9. Dynamic pressure sensitivity determination with Mach number method

    Science.gov (United States)

    Sarraf, Christophe; Damion, Jean-Pierre

    2018-05-01

    Measurements of pressure in fast transient conditions are often performed even if the dynamic characteristic of the transducer are not traceable to international standards. Moreover, the question of a primary standard in dynamic pressure is still open, especially for gaseous applications. The question is to improve dynamic standards in order to respond to expressed industrial needs. In this paper, the method proposed in the EMRP IND09 ‘Dynamic’ project, which can be called the ‘ideal shock tube method’, is compared with the ‘collective standard method’ currently used in the Laboratoire de Métrologie Dynamique (LNE/ENSAM). The input is a step of pressure generated by a shock tube. The transducer is a piezoelectric pressure sensor. With the ‘ideal shock tube method’ the sensitivity of a pressure sensor is first determined dynamically. This method requires a shock tube implemented with piezoelectric shock wave detectors. The measurement of the Mach number in the tube allows an evaluation of the incident pressure amplitude of a step using a theoretical 1D model of the shock tube. Heat transfer, other actual effects and effects of the shock tube imperfections are not taken into account. The amplitude of the pressure step is then used to determine the sensitivity in dynamic conditions. The second method uses a frequency bandwidth comparison to determine pressure at frequencies from quasi-static conditions, traceable to static pressure standards, to higher frequencies (up to 10 kHz). The measurand is also a step of pressure generated by a supposed ideal shock tube or a fast-opening device. The results are provided as a transfer function with an uncertainty budget assigned to a frequency range, also deliverable frequency by frequency. The largest uncertainty in the bandwidth of comparison is used to trace the final pressure step level measured in dynamic conditions, owing that this pressure is not measurable in a steady state on a shock tube. A reference

  10. Simultaneous determination of tyrosine, phenylalanine and deoxyguanosine oxidation products by liquid chromatography-tandem mass spectrometry as non-invasive biomarkers for oxidative damage

    NARCIS (Netherlands)

    Orhan, Hilmi; Vermeulen, Nico P E; Tump, Cornelis; Zappey, Herman; Meerman, John H N

    2004-01-01

    We developed an isotope dilution HPLC-atmospheric pressure chemical ionization-tandem mass spectrometry (HPLC-APCI-MS/MS) method for the simultaneous determination of p-tyrosine, phenylalanine, o,o'-dityrosine, m-tyrosine, o-tyrosine, 3-chlorotyrosine and 3-nitrotyrosine and

  11. Simultaneous determination of eight common odors in natural water body using automatic purge and trap coupled to gas chromatography with mass spectrometry.

    Science.gov (United States)

    Deng, Xuwei; Liang, Gaodao; Chen, Jun; Qi, Min; Xie, Ping

    2011-06-17

    Production and fate of taste and odor (T&O) compounds in natural waters are a pressing environmental issue. Simultaneous determination of these complex compounds (covering a wide range of boiling points) has been difficult. A simple and sensitive method for the determination of eight malodors products of cyanobacterial blooms was developed using automatic purge and trap (P&T) coupled with gas chromatography-mass spectrometry (GC-MS). This extraction and concentration technique is solvent-free. Dimethylsulfide (DMS), dimethyltrisulfide (DMTS), 2-isopropyl-3-methoxypyrazine (IPMP), 2-isobutyl-3-methoxypyrazine (IBMP), 2-methylisoborneol (MIB), β-cyclocitral, geosmin (GSM) and β-ionone were separated within 15.3 min. P&T uses trap #07 and high-purity nitrogen purge gas. The calibration curves of the eight odors show good linearity in the range of 1-500 ng/L with a correlation coefficient above 0.999 (levels=8) and with residuals ranging from approximately 83% to 124%. The limits of detection (LOD) (S/N=3) are all below 1.5 ng/L that of GSM is even lower at 0.08 ng/L. The relative standard deviations (RSD) are between 3.38% and 8.59% (n=5) and recoveries of the analytes from water samples of a eutrophic lake are between 80.54% and 114.91%. This method could be widely employed for monitoring these eight odors in natural waters. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. [Simultaneous determination of principal components and related substances of raw material drug of ammonium glycyrrhizinate by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Zhao, Yanyan; Liu, Liyan; Han, Yuanyuan; Li, Yueqiu; Wang, Yan; Shi, Minjian

    2013-09-01

    An analytical method for the simultaneous determination of 18alpha-glycyrrhizic acid, 18beta-glycyrrhizinic acid, related substances A and B and drug quality standard by reversed-phase high performance liquid chromatography (RP-HPLC) was established. The assay was carried out on a Durashell-C18 column (250 mm x 4.6 mm, 5 microm) with 10 mmol/L ammonium perchlorate (the pH value was adjusted to 8.20 with ammonia)-methanol (48:52, v/v) as mobile phase at a flow rate of 0.80 mL/min, and the detection wavelength was set at 254 nm. The column temperature was 50 degrees C and the injection volume was 10 microL. Under the separation conditions, the calibration curves of the analytes showed good linearities within the mass concentrations of 0.50 -100 mg/L (r > 0.999 9). The detection limits for 18alpha-glycyrrhizic acid, 18beta-glycyrrhizinic acid, related substances A and B were 0.15, 0.10, 0.10, 0.15 mg/L, respectively. The average recoveries were between 97.32% and 99.33% (n = 3) with the relative standard deviations (RSDs) between 0.05% and 1.06%. The method is sensitive, reproducible, and the results are accurate and reliable. The method can be used for the determination of principal components and related substances of ammonium glycyrrhizinate for the quality control of raw material drug of ammonium glycyrrhizinate.

  13. Phase Sensitive Amplification using Parametric Processes in Optical Fibers

    DEFF Research Database (Denmark)

    Kang, Ning

    . Further, phase sensitive parametric processes in a nano-engineered silicon waveguide have been measured experimentally for the first time. Numerical optimizations show that with reduced waveguide propagation loss and reduced carrier life time, larger signal phase sensitive extinction ratio is achievable......Phase sensitive amplification using the parametric processes in fiber has the potential of delivering high gain and broadband operation with ultralow noise. It is able to regenerate both amplitude and phase modulated signals, simultaneously, with the appropriate design. This thesis concerns...... types. The regeneration capability of PSAs on phase encoded signal in an optical link has been optimized. Flat-top phase sensitive profile has been synthesized. It is able to provide simultaneous amplitude and phase noise squeezing, with enhanced phase noise margin compared to conventional designs...

  14. Simultaneous determination of phenytoin, carbamazepine, and 10,11-carbamazepine epoxide in human plasma by high-performance liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Bhatti, M M; Hanson, G D; Schultz, L

    1998-03-01

    The Bioanalytical Chemistry Department at the Madison facility of Covance Laboratories, has developed and validated a simple and sensitive method for the simultaneous determination of phenytoin (PHT), carbamazepine (CBZ) and 10,11-carbamazepine epoxide (CBZ-E) in human plasma by high-performance liquid chromatography with 10,11 dihydrocarbamazepine as the internal standard. Acetonitrile was added to plasma samples containing PHT, CBZ and CBZ-E to precipitate the plasma proteins. After centrifugation, the acetonitrile supernatant was transferred to a clean tube and evaporated under N2. The dried sample extract was reconstituted in 0.4 ml of mobile phase and injected for analysis by high-performance liquid chromatography. Separation was achieved on a Spherisorb ODS2 analytical column with a mobile phase of 18:18:70 acetonitrile:methanol:potassium phosphate buffer. Detection was at 210 nm using an ultraviolet detector. The mean retention times of CBZ-E, PHT and CBZ were 5.8, 9.9 and 11.8 min, respectively. Peak height ratios were fit to a least squares linear regression algorithm with a 1/(concentration)2 weighting. The method produces acceptable linearity, precision and accuracy to a minimum concentration of 0.050 micrograms ml-1 in human plasma. It is also simple and convenient, with no observable matrix interferences.

  15. Simultaneous determination of 30 hormones illegally added to anti-ageing functional foods using UPLC-MS/MS coupled with SPE clean-up.

    Science.gov (United States)

    He, Xiaoqin; Xi, Cunxian; Tang, Bobin; Wang, Guomin; Chen, Dongdong; Peng, Tao; Mu, Zhaode

    2014-01-01

    A novel analytical method employing solid-phase extraction (SPE) coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 30 hormones in anti-ageing functional foods (capsules, powders and tablets). The analytes were extracted with acetic acid-acetonitrile (1-99 v/v), methanol and acetone, respectively. The extract was purified using a combined column, followed by analyte detection with electrospray ionisation in positive- or negative-ion modes. The results indicated that the 30 compounds had good linear correlations in the range of 1-1000 μg kg⁻¹, and the correlation coefficients were above 0.99. The limits of detection (LOD) and limits of quantification (LOQ) were 0.03-2 and 0.1-5 μg kg⁻¹, respectively. The average recovery of 30 compounds at the three spiked levels varied from 74.7% to 124.1%, and the relative standard deviation (RSD) was 2.4-15.0%. This method was applied to the analysis of hormones in 14 real samples of which seven hormones (such as estrone, dienestrol) were detected in four samples, but the remainder of the hormones were not detected. The developed method is sensitive, efficient, reliable and applicable to real samples.

  16. A validated high-performance liquid chromatography method with diode array detection for simultaneous determination of nine flavonoids in Senecio cannabifolius Less.

    Science.gov (United States)

    Niu, Tian-Zeng; Zhang, Yu-Wei; Bao, Yong-Li; Wu, Yin; Yu, Chun-Lei; Sun, Lu-Guo; Yi, Jing-Wen; Huang, Yan-Xin; Li, Yu-Xin

    2013-03-25

    A reversed phase high performance liquid chromatography method coupled with a diode array detector (HPLC-DAD) was developed for the first time for the simultaneous determination of 9 flavonoids in Senecio cannabifolius, a traditional Chinese medicinal herb. Agilent Zorbax SB-C18 column was used at room temperature and the mobile phase was a mixture of acetonitrile and 0.5% formic acid (v/v) in water in the gradient elution mode at a flow-rate of 1.0mlmin(-1), detected at 360nm. Validation of this method was performed to verify the linearity, precision, limits of detection and quantification, intra- and inter-day variabilities, reproducibility and recovery. The calibration curves showed good linearities (R(2)>0.9995) within the test ranges. The relative standard deviation (RSD) of the method was less than 3.0% for intra- and inter-day assays. The samples were stable for at least 96h, and the average recoveries were between 90.6% and 102.5%. High sensitivity was demonstrated with detection limits of 0.028-0.085μg/ml for flavonoids. The newly established HPLC method represents a powerful technique for the quality assurance of S. cannabifolius. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. A novel technique for the simultaneous determination of 210Pb and 210Po using a crown ether

    International Nuclear Information System (INIS)

    Vajda, N.; LaRosa, J.; Zeisler, R.; Danesi, P.; Kis-Benedek, Gy.

    1997-01-01

    A simple radiochemical procedure has been developed to separate lead and polonium simultaneously from different environmental and biological materials. After adding 208 Po tracer and lead carrier, samples are decomposed using mineral acids. Lead and polonium are selectively retained from 2M HCl solution by the bis-4,4'(5')-t-butyl-cyclohexano-18-crown-6-ether; polonium is stripped with 6 M HNO 3 while lead is stripped with 6 M HCL solution. A polonium source is prepared by spontaneous deposition onto a silver disk. The activity concentration of 210 Po is determined by isotope dilution alpha spectrometry. Lead is precipitated as oxalate; the chemical recovery is determined by gravimetry. The activity concentration of 210 Pb is calculated from the liquid scintillation spectrum. (author)

  18. A sensor of a polyoxometalate and Au–Pd alloy for simultaneously detection of dopamine and ascorbic acid

    International Nuclear Information System (INIS)

    Zhou, Chunlei; Li, Shuang; Zhu, Wei; Pang, Haijun; Ma, Huiyuan

    2013-01-01

    A composite film based on K 8 P 2 W 16 V 2 O 62 ·18H 2 O decorated by Au–Pd nanoparticles was prepared by the layer-by-layer self-assembly method. This composite film exhibits enhanced electrocatalytic performance, repeatability and long-term stability for the simultaneous determination of dopamine and ascorbic acid at biological pH (pH 7.0). The proposed electrochemical sensing film for simultaneous detecting dopamine and ascorbic acid shows rather low detection limit of 8.3 × 10 −7 and 4.3 × 10 −7 M and a linear response range from 2.1 × 10 −6 to 2.06 × 10 −3 M and 1.2 × 10 −6 to 1.61 × 10 −3 M, as well as no interference from the common interfering species at an applied potential. -- Abstract: A novel composite film based on Dawson-type phosphovanadotungstate K 8 P 2 W 16 V 2 O 62 ·18H 2 O (P 2 W 16 V 2 ) decorated by Au–Pd alloy nanoparticles (Au–Pd) was fabricated on quartz, silicon and ITO using the layer-by-layer self-assembly method. The composite film was characterized by UV–vis spectroscopy, X-ray photoelectron spectra, atomic force microscopy, Scanning electronic microscope, cyclic voltammetry and differential pulse voltammetry. The composite film can be employed for sensitive and simultaneous determination of dopamine and ascorbic acid at biological pH (pH 7.0). Linear analytical curves were obtained in the ranges from 2.1 × 10 −6 to 2.06 × 10 −3 M and 1.2 × 10 −6 to 1.61 × 10 −3 M for dopamine and ascorbic acid by DPV methods, respectively. The low detection limit for dopamine and ascorbic acid were 8.3 × 10 −7 and 4.3 × 10 −7 M, as well as no interference was observed from the common interfering species such as glucose, uric acid, L-cysteine, CH 3 OH, CH 3 CH 2 OH and H 2 O 2 . The composite film was used for dopamine and ascorbic acid determinations in real samples with satisfactory results. With high sensitivity and selectivity, the proposed electrochemical sensor would provide a simple method for

  19. A stimuli-responsive fluorescence platform for simultaneous determination of d-isoascorbic acid and Tartaric acid based on Maillard reaction product.

    Science.gov (United States)

    Zhao, Yanmei; Yuan, Haiyan; Zhang, Xinling; Yang, Jidong

    2018-05-05

    An activatable fluorescence monitoring platform based on a novel Maillard reaction product from d-glucose and L-arginine was prepared through a facile one-pot approach and applied for simultaneous detection of d-isoascorbic acid and tartaric acid. In this work, the new Maillard reaction product GLA was first obtained, and its fluorescence intensity can be effectively quenched by KMnO 4 , resulting from a new complex (GLA-KMnO 4 ) formation between GLA and KMnO 4 . Upon addition of d-isoascorbic acid or tartaric acid, an enhanced fluorescence was observed under the optimumed experimental conditions, indicating a stimuli-responsive fluorescence turn on platform for d-isoascorbic acid or tartaric acid can be developed. The corresponding experimental results showed that this turn on fluorescence sensing platform has a high sensitivity for d-isoascorbic acid or tartaric acid, because the detection limits were 5.9μM and 21.5μM, respectively. Additionally, this proposed sensing platform was applied to simultaneously detection of d-isoascorbic acid and tartaric acid in real tap water samples with satisfactory results. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Sequential Spectrophotometric Method for the Simultaneous Determination of Amlodipine, Valsartan, and Hydrochlorothiazide in Coformulated Tablets

    Directory of Open Access Journals (Sweden)

    Hany W. Darwish

    2013-01-01

    Full Text Available A new, simple and specific spectrophotometric method was developed and validated in accordance with ICH guidelines for the simultaneous estimation of Amlodipine (AML, Valsartan (VAL, and Hydrochlorothiazide (HCT in their ternary mixture. In this method three techniques were used, namely, direct spectrophotometry, ratio subtraction, and isoabsorptive point. Amlodipine (AML was first determined by direct spectrophotometry and then ratio subtraction was applied to remove the AML spectrum from the mixture spectrum. Hydrochlorothiazide (HCT could then be determined directly without interference from Valsartan (VAL which could be determined using the isoabsorptive point theory. The calibration curve is linear over the concentration ranges of 4–32, 4–44 and 6–20 μg/mL for AML, VAL, and HCT, respectively. This method was tested by analyzing synthetic mixtures of the above drugs and was successfully applied to commercial pharmaceutical preparation of the drugs, where the standard deviation is <2 in the assay of raw materials and tablets. The method was validated according to the ICH guidelines and accuracy, precision, repeatability, and robustness were found to be within the acceptable limits.

  1. Sensitive spectrophotometric methods for determination of some organophosphorus pesticides in vegetable samples

    Directory of Open Access Journals (Sweden)

    MAGDA A. AKL

    2010-03-01

    Full Text Available Three rapid, simple, reproducible and sensitive spectrophotometric methods (A, B and C are described for the determination of two organophosphorus pesticides, (malathion and dimethoate in formulations and vegetable samples. The methods A and B involve the addition of an excess of Ce4+ into sulphuric acid medium and the determination of the unreacted oxidant by decreasing the red color of chromotrope 2R (C2R at a suitable lmax = 528 nm for method A, or a decrease in the orange pink color of rhodamine 6G (Rh6G at a suitable lmax = = 525 nm. The method C is based on the oxidation of malathion or dimethoate with the slight excess of N-bromosuccinimide (NBS and the determination of unreacted oxidant by reacting it with amaranth dye (AM in hydrochloric acid medium at a suitable lmax = 520 nm. A regression analysis of Beer-Lambert plots showed a good correlation in the concentration range of 0.1-4.2 μg mL−1. The apparent molar absorptivity, Sandell sensitivity, the detection and quantification limits were calculated. For more accurate analysis, Ringbom optimum concentration ranges are 0.25-4.0 μg mL−1. The developed methods were successfully applied to the determination of malathion, and dimethoate in their formulations and environmental vegetable samples.

  2. Determinação simultânea de precursores de serotonina - triptofano e 5-hidroxitriptofano - em café Simultaneous determination of serotonin precursors - tryptophan and 5-hidroxytryptophan - in coffee

    Directory of Open Access Journals (Sweden)

    Ana Carolina C. L. Martins

    2010-01-01

    Full Text Available Epidemiological studies attributed positive effects in the central nervous system (CNS to coffee. Among possible active constituents, serotonin, a neurotransmitter in the CNS, is present; but dietary sources do not cross the blood-brain barrier. Tryptophan and 5-hidroxytryptophan (5-HTP are serotonin precursors and can affect brain concentrations. An ion-pair-HPLC, post-column derivatization with o-phthalaldehyde and fluorimetric detection before and after hydrolysis with NaOH and extraction with methanol:water was developed for the simultaneous determination of these compounds. It was selective, sensitive (LOD = 0.3 and 0.2 μg/mL, precise (91.3 and 94.2% recovery for tryptophan and 5-HTP, respectively, and linear from 0.3 to 40 μg/mL for both compounds. It was applied to green and roasted arabica and robusta coffees.

  3. Alterations in audiovisual simultaneity perception in amblyopia.

    Science.gov (United States)

    Richards, Michael D; Goltz, Herbert C; Wong, Agnes M F

    2017-01-01

    Amblyopia is a developmental visual impairment that is increasingly recognized to affect higher-level perceptual and multisensory processes. To further investigate the audiovisual (AV) perceptual impairments associated with this condition, we characterized the temporal interval in which asynchronous auditory and visual stimuli are perceived as simultaneous 50% of the time (i.e., the AV simultaneity window). Adults with unilateral amblyopia (n = 17) and visually normal controls (n = 17) judged the simultaneity of a flash and a click presented with both eyes viewing. The signal onset asynchrony (SOA) varied from 0 ms to 450 ms for auditory-lead and visual-lead conditions. A subset of participants with amblyopia (n = 6) was tested monocularly. Compared to the control group, the auditory-lead side of the AV simultaneity window was widened by 48 ms (36%; p = 0.002), whereas that of the visual-lead side was widened by 86 ms (37%; p = 0.02). The overall mean window width was 500 ms, compared to 366 ms among controls (37% wider; p = 0.002). Among participants with amblyopia, the simultaneity window parameters were unchanged by viewing condition, but subgroup analysis revealed differential effects on the parameters by amblyopia severity, etiology, and foveal suppression status. Possible mechanisms to explain these findings include visual temporal uncertainty, interocular perceptual latency asymmetry, and disruption of normal developmental tuning of sensitivity to audiovisual asynchrony.

  4. Alterations in audiovisual simultaneity perception in amblyopia.

    Directory of Open Access Journals (Sweden)

    Michael D Richards

    Full Text Available Amblyopia is a developmental visual impairment that is increasingly recognized to affect higher-level perceptual and multisensory processes. To further investigate the audiovisual (AV perceptual impairments associated with this condition, we characterized the temporal interval in which asynchronous auditory and visual stimuli are perceived as simultaneous 50% of the time (i.e., the AV simultaneity window. Adults with unilateral amblyopia (n = 17 and visually normal controls (n = 17 judged the simultaneity of a flash and a click presented with both eyes viewing. The signal onset asynchrony (SOA varied from 0 ms to 450 ms for auditory-lead and visual-lead conditions. A subset of participants with amblyopia (n = 6 was tested monocularly. Compared to the control group, the auditory-lead side of the AV simultaneity window was widened by 48 ms (36%; p = 0.002, whereas that of the visual-lead side was widened by 86 ms (37%; p = 0.02. The overall mean window width was 500 ms, compared to 366 ms among controls (37% wider; p = 0.002. Among participants with amblyopia, the simultaneity window parameters were unchanged by viewing condition, but subgroup analysis revealed differential effects on the parameters by amblyopia severity, etiology, and foveal suppression status. Possible mechanisms to explain these findings include visual temporal uncertainty, interocular perceptual latency asymmetry, and disruption of normal developmental tuning of sensitivity to audiovisual asynchrony.

  5. A gas sensor array for the simultaneous detection of multiple VOCs.

    Science.gov (United States)

    Zhang, Yumin; Zhao, Jianhong; Du, Tengfei; Zhu, Zhongqi; Zhang, Jin; Liu, Qingju

    2017-05-16

    Air quality around the globe is declining and public health is seriously threatened by indoor air pollution. Typically, indoor air pollutants are composed of a series of volatile organic compounds (VOCs) that are generally harmful to the human body, especially VOCs with low molecular weights (less than 100 Da). Moreover, in some situations, more than one type of VOC is present; thus, a device that can detect one or more VOCs simultaneously would be most beneficial. Here, we synthesized a sensor array with 4 units to detect 4 VOCs: acetone (unit 1), benzene (unit 2), methanol (unit 3) and formaldehyde (unit 4) simultaneously. All units were simultaneously exposed to 2.5 ppm of all four VOCs. The sensitivity of unit 1 was 14.67 for acetone and less than 2.54 for the other VOCs. The sensitivities of units 2, 3 and 4 to benzene, methanol and formaldehyde were 2 18.64, 20.98 and 17.26, respectively, and less than 4.01 for the other VOCs. These results indicated that the sensor array exhibited good selectivity and could be used for the real-time monitoring of indoor air quality. Thus, this device will be useful in situations requiring the simultaneous detection of multiple VOCs.

  6. Simultaneous determination of some common food dyes in commercial products by digital image analysis

    Directory of Open Access Journals (Sweden)

    Mohammad-Hossein Sorouraddin

    2015-09-01

    Full Text Available A simple and relatively fast image-analysis method using digital images, obtained with a flatbed scanner, has been described. The method was used for the simultaneous determination of four common food dyes, namely, carmoisine, brilliant blue, sunset yellow, and quinoline yellow, in binary mixtures in commercial products without a need for any prior separation steps. The results obtained were validated against a standard high-performance liquid chromatography method and a good agreement was obtained. The parameters affecting the experimental results were optimized. Under the optimal conditions, the method provided acceptable linear ranges (20–250 mg/L with correlation coefficients higher than 0.998, suitable precision (relative standard deviation ≤ 4.5%, and limits of detection between 4.82 and 8.05 mg/L.

  7. Simultaneous determination of devolatilization and char burnout times during fluidized bed combustion of coal

    International Nuclear Information System (INIS)

    Christofiedes, N.; Brown, R.C.

    1992-01-01

    In this paper, the authors investigate a method for simultaneous determination of devolatilization and char burnout times based on the analysis of CO 2 emissions from a fluidized bed combustor. The technique is non-intrusive and can be performed under realistic combustion conditions. The authors' method involves batching single-size coal samples in a fluidized bed combustor that is heated with propane gas or other fuel. Carbon dioxide profiles versus time for the batch tests are analyzed with a linear model to obtain characteristic time constants for coal devolatilization and char combustion which can be related to total devolatilization time and burnout time for a coal sample. The authors' approach does not require special sample preparation, can be performed in actual combustion equipment and employs standard boiler instrumentation

  8. Simultaneous determination of multi-mycotoxins in palm kernel cake (PKC) using liquid chromatography-tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Yibadatihan, S; Jinap, S; Mahyudin, N A

    2014-01-01

    Palm kernel cake (PKC) is a useful source of protein and energy for livestock. Recently, it has been used as an ingredient in poultry feed. Mycotoxin contamination of PKC due to inappropriate handling during production and storage has increased public concern about economic losses and health risks for poultry and humans. This concern has accentuated the need for the evaluation of mycotoxins in PKC. Furthermore, a method for quantifying mycotoxins in PKC has so far not been established. The aims of this study were therefore (1) to develop a method for the simultaneous determination of mycotoxins in PKC and (2) to validate and verify the method. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using an electrospray ionisation interface (ESI) in both positive- and negative-ion modes was developed for the simultaneous determination of aflatoxins (AFB₁, AFB₂, AFG₁ and AFG₂), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB₁ and FB₂), T-2 and HT-2 toxin in PKC. An optimum method using a 0.2 ml min⁻¹ flow rate, 0.2% formic acid in aqueous phase, 10% organic phase at the beginning and 90% organic phase at the end of the gradient was achieved. The extraction of mycotoxins was performed using a solvent mixture of acetonitrile-water-formic acid (79:20:1, v/v) without further clean-up. The mean recoveries of mycotoxins in spiked PKC samples ranged from 81% to 112%. Limits of detection (LODs) and limits of quantification (LOQs) for mycotoxin standards and PKC samples ranged from 0.02 to 17.5 μg kg⁻¹ and from 0.06 to 58.0 μg kg⁻¹, respectively. Finally, the newly developed method was successfully applied to PKC samples. The results illustrated the fact that the method is efficient and accurate for the simultaneous multi-mycotoxin determination in PKC, which can be ideal for routine analysis.

  9. Development and validation of High-performance Thin-layer Chromatography Method for Simultaneous Determination of Polyphenolic Compounds in Medicinal Plants.

    Science.gov (United States)

    Jayachandran Nair, C V; Ahamad, Sayeed; Khan, Washim; Anjum, Varisha; Mathur, Rajani

    2017-12-01

    Quantitative standardization of plant-based products is challenging albeit essential to maintain their quality. This study aims to develop and validate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of rutin (Ru), quercetin (Qu), and gallic acid (Ga) from Psidium guajava Linn. (PG) and Aegle marmelos (L.) Correa. (AM) and correlate with antioxidant activity. The stock solution (1 mg/mL) of standard Ru, Qu, and Ga in methanol: Water (1:1) was serially diluted and spotted (5 μL) on slica gel 60 F 254 thin-layer chromatography plates. Toluene: Ethyl acetate: Formic acid: Methanol (3:4:0.8:0.7, v/v/v) was selected as mobile phase for analysis at 254 nm. Hydroalcoholic (1:1) extracts of leaves of PG and AM were fractionated and similarly analyzed. Antioxidant activity was also determined using 2, 2-diphenyl-1-picrylhydrazyl assay. The developed method was robust and resolved Ru, Qu, and Ga at R f 0.08 ± 0.02, 0.76 ± 0.01, and 0.63 ± 0.02, respectively. The intra-day, interday precision, and interanalyst were limit of detection and limit of quantification for Ru, Qu, and Ga were 4.51, 4.2, 5.27, and 13.67, 12.73, 15.98 ng/spot, respectively. Antioxidant activity (Log 50% inhibition) of PG and AM was 4.947 ± 0.322 and 6.498 ± 0.295, respectively. The developed HPTLC method was rapid, accurate, precise, reproducible, and specific for the simultaneous estimation of Ru, Qu, and Ga. HPTLC method for simultaneous determination and quantification of Rutin, Quercetin and Gallic acid, is reported for quality control of herbal drugs. Abbreviations Used: A: Aqueous fraction; AM: Aegle marmelos L. Correa; B: Butanol fraction; C: Chloroform fraction; EA: Ethyl acetate fraction; Ga: Gallic acid; H: Hexane fraction; HA: Hydroalcoholic extract; HPTLC: High-performance thin-layer chromatography; PG: Psidium guajava ; Qu: Quercetin; Ru: Rutin.

  10. Double-wavelength overlapping resonance Rayleigh scattering technique for the simultaneous quantitative analysis of three β-adrenergic blockade

    Science.gov (United States)

    Tan, Xuanping; Yang, Jidong; Li, Qin; Yang, Qiong; Shen, Yizhong

    2016-05-01

    Four simple and accurate spectrophotometric methods were proposed for the simultaneous determination of three β-adrenergic blockade, e.g. atenolol, metoprolol and propranolol. The methods were based on the reaction of the three drugs with erythrosine B (EB) in a Britton-Robinson buffer solution at pH 4.6. EB could combine with the drugs to form three ion-association complexes, which resulted in the resonance Rayleigh scattering (RRS) intensity that is enhanced significantly with new RRS peaks that appeared at 337 nm and 370 nm, respectively. In addition, the fluorescence intensity of EB was also quenched. The enhanced scattering intensities of the two peaks and the fluorescence quenched intensity of EB were proportional to the concentrations of the drugs, respectively. What is more, the RRS intensity overlapped with the double-wavelength of 337 nm and 370 nm (so short for DW-RRS) was also proportional to the drugs concentrations. So, a new method with highly sensitive for simultaneous determination of three bisoprolol drugs was established. Finally, the optimum reaction conditions, influencing factors and spectral enhanced mechanism were investigated. The new DW-RRS method has been applied to simultaneously detect the three β-blockers in fresh serum with satisfactory results.

  11. Determination of IgE antibodies to the benzylpenicilloyl determinant: a comparison of the sensitivity and specificity of three radio allergo sorbent test methods.

    Science.gov (United States)

    Garcia, J J; Blanca, M; Moreno, F; Vega, J M; Mayorga, C; Fernandez, J; Juarez, C; Romano, A; de Ramon, E

    1997-01-01

    The quantitation of in vitro IgE antibodies to the benzylpenicilloyl determinant (BPO) is a useful tool for evaluating suspected penicillin allergic subjects. Although many different methods have been employed, few studies have compared their diagnostic specificity and sensitivity. In this study, the sensitivity and specificity of three different radio allergo sorbent test (RAST) methods for quantitating specific IgE antibodies to the BPO determinant were compared. Thirty positive control sera (serum samples from penicillin allergic subjects with a positive clinical history and a positive penicillin skin test) and 30 negative control sera (sera from subjects with no history of penicillin allergy and negative skin tests) were tested for BPO-specific IgE antibodies by RAST using three different conjugates coupled to the solid phase: benzylpenicillin conjugated to polylysine (BPO-PLL), benzylpenicillin conjugated to human serum albumin (BPO-HSA), and benzylpenicillin conjugated to an aminospacer (BPO-SP). Receiver operator control curves (ROC analysis) were carried out by determining different cut-off points between positive and negative values. Contingence tables were constructed and sensitivity, specificity, negative predictive values (PV-), and positive predictive values (PV+) were calculated. Pearson correlation coefficients (r) and intraclass correlation coefficients (ICC) were determined and the differences between methods were compared by chi 2 analysis. Analysis of the areas defined by the ROC curves showed statistical differences among the three methods. When cut-off points for optimal sensitivity and specificity were chosen, the BPO-HSA assay was less sensitive and less specific and had a lower PV- and PV+ than the BPO-PLL and BPO-SP assays. Assessment of r and ICC indicated that the correlation was very high, but the concordance between the PLL and SP methods was higher than between the PLL and HSA or SP and HSA methods. We conclude that for quantitating Ig

  12. Simultaneous determination of eugenol, isoeugenol and methyleugenol in fish fillet using gas chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Ke, Changliang; Liu, Qi; Li, Liudong; Chen, Jiewen; Wang, Xunuo; Huang, Ke

    2016-09-15

    Gas chromatography (GC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) operated in electron ionization mode (EI) has been shown to have advantages in the trace analysis of chemical compounds. Employing the instrument, a method has been built to simultaneously determine eugenol, isoeugenol' and methyleugenol, which have been widely used as fish anesthetic, in the fish fillet. Procedure for the sample preparation was achieved by using hexane extraction followed by phenyl solid phase extraction (SPE) cleanup, which was free of such steps as rotary evaporation and nitrogen blowing by taking the volatility of eugenol and its isomers into consideration. The method was validated by conducting recovery studies on fortified fish fillet samples at four concentrations. The linearity in the range of 5-500μg·L(-1) was forced through the origin giving a coefficient of determination (r(2)) greater than 0.9982. Limits of detection (LODs) for eugenol, isoeugenol' and methyleugenol were 0.4, 1.2' and 0.2μg·kg(-1), respectively. The limits of quantification (LOQs) were 1.2, 4' and 0.7μg·kg(-1) for eugenol, isoeugenol' and methyleugenol, respectively. The recoveries for eugenol and its isomers ranged from 76.4 to 99.9% with relative standard deviations (RSD) in a range from 2.18 to 15.5%. This method is quick, simple and suitable for determining the residues of eugenol, isoeugenol and methyleugenol simultaneously in batch samples of fish fillet. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Simultaneous alcohol and cannabis expectancies predict simultaneous use

    Directory of Open Access Journals (Sweden)

    Earleywine Mitch

    2006-10-01

    Full Text Available Abstract Background Simultaneous use of alcohol and cannabis predicts increased negative consequences for users beyond individual or even concurrent use of the two drugs. Given the widespread use of the drugs and common simultaneous consumption, problems unique to simultaneous use may bear important implications for many substance users. Cognitive expectancies offer a template for future drug use behavior based on previous drug experiences, accurately predicting future use and problems. Studies reveal similar mechanisms underlying both alcohol and cannabis expectancies, but little research examines simultaneous expectancies for alcohol and cannabis use. Whereas research has demonstrated unique outcomes associated with simultaneous alcohol and cannabis use, this study hypothesized that unique cognitive expectancies may underlie simultaneous alcohol and cannabis use. Results: This study examined a sample of 2600 (66% male; 34% female Internet survey respondents solicited through advertisements with online cannabis-related organizations. The study employed known measures of drug use and expectancies, as well as a new measure of simultaneous drug use expectancies. Expectancies for simultaneous use of alcohol and cannabis predicted simultaneous use over and above expectancies for each drug individually. Discussion Simultaneous expectancies may provide meaningful information not available with individual drug expectancies. These findings bear potential implications on the assessment and treatment of substance abuse problems, as well as researcher conceptualizations of drug expectancies. Policies directing the treatment of substance abuse and its funding ought to give unique consideration to simultaneous drug use and its cognitive underlying factors.

  14. Simultaneous determination of gallic acid and gentisic acid in organic anion transporter expressing cells by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wang, Li; Halquist, Matthew S; Sweet, Douglas H

    2013-10-15

    In order to elucidate the role of organic anion transporters (OATs) in the renal elimination of gallic acid and gentisic acid, a new, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous determination of gallic acid and gentisic acid in cell lysate, using Danshensu as the internal standard (IS). After a simple liquid-liquid extraction, the analytes were detected in negative ESI mode using selected reaction monitoring. The precursor-to-product ion transitions (m/z) were 169.0→125.0, 153.1→108.0, and 196.8→135.2 for gallic acid, gentisic acid, and the IS, respectively. Chromatographic separation was achieved on a C18 column using mobile phases consisting of water with 0.1% acetic acid (A) and acetonitrile with 0.05% formic acid. (B) The total run time was 3min and calibration curves were linear over the concentrations of 0.33-2400ng/mL for both compounds (r(2)>0.995). Good precision (between 3.11% and 14.1% RSD) and accuracy (between -12.7% and 11% bias) was observed for quality controls at concentrations of 0.33 (lower limit of quantification), 1, 50, and 2000ng/mL. The mean extraction recovery of gallic acid and gentisic acid was 80.7% and 83.5%, respectively. Results from post-column infusion and post-extraction methods indicated that the analytical method exhibited negligible matrix effects. Finally, this validated assay was successfully applied in a cellular uptake study to determine the intracellular concentrations of gallic acid and gentisic acid in OAT expressing cells. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Validation of a liquid chromatography method for the simultaneous determination of sulfadimethoxine and trimethoprim and application to a stability study.

    Science.gov (United States)

    Louati, K; Mistiri, F; Kallel, M; Safta, F

    2010-03-01

    A liquid chromatography method is described for the simultaneous determination of sulfadimetoxine and trimethoprim from a veterinary formulation at the proportion of 187 mg and 40 mg respectively in presence of some excipient. The solution was subjected to different International Conference On Harmonisation prescribed stress conditions (hydrolysis, oxidation and photolysis). A stability-indicating high-performance liquid chromatography method was developed for the analysis of active substances in presence of their major degradation products. It involved a Knauer Eurospher C18 thermostated column at 25 degrees C, and 9.57 mM phosphate buffer (pH adjusted to 2.0 with orthophosphoric acid)-acetonitrile (70:30 v/v) as mobile phase. The mobile phase flow rate and sample volume injected were 1.2 mL/min and 20 microL, respectively. The selected wavelength for the determination was 248 nm. The method was validated for linearity, precision, accuracy and specificity, and then applied to a stability study of sulfadimetoxine and trimethoprim in the veterinary solution packaged in high density polyethylene plastic bottles of 1 L and 100 mL thermosealed and no thermosealed and corked by a white cap, at both accelerated and long-term conditions required by the International Conference On Harmonisation. The method developed, which separates all of the most degradation products formed under variety of conditions, proved to be simple, accurate, precise and specific. The results of the stress degradation show that the solution is more sensitive to hydrolysis. The stability studies carried out on three batches of each presentation show that the finished product remains stable for six months. Copyright 2010 Elsevier Masson SAS. All rights reserved.

  16. A "three-in-one" sample preparation method for simultaneous determination of B-group water-soluble vitamins in infant formula using VitaFast(®) kits.

    Science.gov (United States)

    Zhang, Heng; Lan, Fang; Shi, Yupeng; Wan, Zhi-Gang; Yue, Zhen-Feng; Fan, Fang; Lin, Yan-Kui; Tang, Mu-Jin; Lv, Jing-Zhang; Xiao, Tan; Yi, Changqing

    2014-06-15

    VitaFast(®) test kits designed for the microbiological assay in microtiter plate format can be applied to quantitative determination of B-group water-soluble vitamins such as vitamin B12, folic acid and biotin, et al. Compared to traditional microbiological methods, VitaFast(®) kits significantly reduce sample processing time and provide greater reliability, higher productivity and better accuracy. Recently, simultaneous determination of vitamin B12, folic acid and biotin in one sample is urgently required when evaluating the quality of infant formulae in our practical work. However, the present sample preparation protocols which are developed for individual test systems, are incompatible with simultaneous determination of several analytes. To solve this problem, a novel "three-in-one" sample preparation method is herein developed for simultaneous determination of B-group water-soluble vitamins using VitaFast(®) kits. The performance of this novel "three-in-one" sample preparation method was systematically evaluated through comparing with individual sample preparation protocols. The experimental results of the assays which employed "three-in-one" sample preparation method were in good agreement with those obtained from conventional VitaFast(®) extraction methods, indicating that the proposed "three-in-one" sample preparation method is applicable to the present three VitaFast(®) vitamin test systems, thus offering a promising alternative for the three independent sample preparation methods. The proposed new sample preparation method will significantly improve the efficiency of infant formulae inspection. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Simultaneous determination of phenolic acids and diterpenoids and their comparative pharmacokinetic study in normal and acute blood stasis rats by UFLC-MS/MS after oral administration of Guan-Xin-Shu-Tong capsules.

    Science.gov (United States)

    Gao, Xun; Mu, Jingqing; Guan, Shaoyi; Li, Qing; Du, Yiyang; Zhang, Huifen; Bi, Kaishun

    2018-01-01

    Guan-Xin-Shu-Tong capsules are one of the well-known and first-line Chinese traditional herbal formula for treating coronary heart disease. A validated and sensitive method via ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) was established to simultaneously determinate five phenolic acids and four diterpenoids in rats in order to investigate their pharmacokinetic profiles firstly. Analytes were extracted by ethyl acetate and determined via multiple reaction monitoring mode in both positive and negative ion modes. The values for limit of quantification were in range of 0.025-1.250ng/ml. Inter- and intra-day precisions were no more than 10.9% with accuracy of -11.0%-10.6%, meanwhile the stable and suitable extraction recoveries were also obtained. And finally such excellent method was used to compare the pharmacokinetics of nine compounds in normal and acute blood stasis rats after oral administration of Guan-Xin-Shu-Tong capsules. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Sequential vs simultaneous revascularization in patients undergoing liver transplantation: A meta-analysis.

    Science.gov (United States)

    Wang, Jia-Zhong; Liu, Yang; Wang, Jin-Long; Lu, Le; Zhang, Ya-Fei; Lu, Hong-Wei; Li, Yi-Ming

    2015-06-14

    We undertook this meta-analysis to investigate the relationship between revascularization and outcomes after liver transplantation. A literature search was performed using MeSH and key words. The quality of the included studies was assessed using the Jadad Score and the Newcastle-Ottawa Scale. Heterogeneity was evaluated by the χ(2) and I (2) tests. The risk of publication bias was assessed using a funnel plot and Egger's test, and the risk of bias was assessed using a domain-based assessment tool. A sensitivity analysis was conducted by reanalyzing the data using different statistical approaches. Six studies with a total of 467 patients were included. Ischemic-type biliary lesions were significantly reduced in the simultaneous revascularization group compared with the sequential revascularization group (OR = 4.97, 95%CI: 2.45-10.07; P simultaneous revascularization group. Although warm ischemia time was prolonged in simultaneous revascularization group (MD = -25.84, 95%CI: -29.28-22.40; P sequential and simultaneous revascularization groups. Assessment of the risk of bias showed that the methods of random sequence generation and blinding might have been a source of bias. The sensitivity analysis strengthened the reliability of the results of this meta-analysis. The results of this study indicate that simultaneous revascularization in liver transplantation may reduce the incidence of ischemic-type biliary lesions and length of stay of patients in the ICU.

  19. Highly sensitive determination of atropine using cobalt oxide nanostructures: Influence of functional groups on the signal sensitivity

    Energy Technology Data Exchange (ETDEWEB)

    Soomro, Razium Ali, E-mail: raziumsoomro@gmail.com [Interface Analysis Centre, School of Physics, University of Bristol, Bristol, BS8 1TL (United Kingdom); National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro, 76080 (Pakistan); Nafady, Ayman [Department of Chemistry, College of Science, King Saud University, Riyadh (Saudi Arabia); Department of Chemistry, Faculty of Science, Sohag University, Sohag (Egypt); Hallam, Keith Richard [Interface Analysis Centre, School of Physics, University of Bristol, Bristol, BS8 1TL (United Kingdom); Jawaid, Sana [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro, 76080 (Pakistan); Al Enizi, Abdullah [Department of Chemistry, College of Science, King Saud University, Riyadh (Saudi Arabia); Sherazi, Syed Tufail Hussain; Sirajuddin [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro, 76080 (Pakistan); Ibupoto, Zafar Hussain [Dr M.A. Kazi Institute of Chemistry, University of Sindh, Jamshoro, 76080 (Pakistan); Willander, Magnus [Department of Science and Technology, Campus Norrkoping, Linkoping University, SE-60174, Norrkoping (Sweden)

    2016-12-15

    This study describes sensitive determination of atropine using glassy carbon electrodes (GCE) modified with Co{sub 3}O{sub 4} nanostructures. The as-synthesised nanostructures were grown using cysteine (CYS), glutathione (GSH) and histidine (HYS) as effective templates under hydrothermal action. The obtained morphologies revealed interesting structural features, including both cavity-based and flower-shaped structures. The as-synthesised morphologies were noted to actively participate in electro-catalysis of atropine (AT) drug where GSH-assisted structures exhibited the best signal response in terms of current density and over-potential value. The study also discusses the influence of functional groups on the signal sensitivity of atropine electro-oxidation. The functionalisation was carried with the amino acids originally used as effective templates for the growth of Co{sub 3}O{sub 4} nanostructures. The highest increment was obtained when GSH was used as the surface functionalising agent. The GSH-functionalised Co{sub 3}O{sub 4}-modified electrode was utilised for the electro-chemical sensing of AT in a concentration range of 0.01–0.46 μM. The developed sensor exhibited excellent working linearity (R{sup 2} = 0.999) and signal sensitivity up to 0.001 μM of AT. The noted high sensitivity of the sensor is associated with the synergy of superb surface architectures and favourable interaction facilitating the electron transfer kinetics for the electro-catalytic oxidation of AT. Significantly, the developed sensor demonstrated excellent working capability when used for AT detection in human urine samples with strong anti-interference potential against common co-existing species, such as glucose, fructose, cysteine, uric acid, dopamine and ascorbic acid. - Highlights: • Template-assisted growth of Co{sub 3}O{sub 4} nanostructures. • Shape-dependent electro-catalysis of atropine. • Effect of functionalisation of signal sensitivity.

  20. Rapid HPLC-MS method for the simultaneous determination of tea catechins and folates.

    Science.gov (United States)

    Araya-Farias, Monica; Gaudreau, Alain; Rozoy, Elodie; Bazinet, Laurent

    2014-05-14

    An effective and rapid HPLC-MS method for the simultaneous separation of the eight most abundant tea catechins, gallic acid, and caffeine was developed. These compounds were rapidly separated within 9 min by a linear gradient elution using a Zorbax SB-C18 packed with sub 2 μm particles. This methodology did not require preparative and semipreparative HPLC steps. In fact, diluted tea samples can be easily analyzed using HPLC-MS as described in this study. The use of mass spectrometry detection for quantification of catechins ensured a higher specificity of the method. The percent relative standard deviation was generally lower than 4 and 7% for most of the compounds tested in tea drinks and tea extracts, respectively. Furthermore, the method provided excellent resolution for folate determination alone or in combination with catechins. To date, no HPLC method able to discriminate catechins and folates in a quick analysis has been reported in the literature.

  1. Resonant tunneling: A method for simultaneous determination of resonance energy and energy eigenvalue

    Energy Technology Data Exchange (ETDEWEB)

    Maiz, F., E-mail: Fethi_maiz@yahoo.fr [King Khalid University, Faculty of Science, Physics Department, P.O. Box 9004, Abha (Saudi Arabia); University of Cartage, Nabeul Engineering Preparatory Institute, Merazka, 8000 Nabeul (Tunisia); Eissa, S.A. [King Khalid University, Faculty of Science, Physics Department, P.O. Box 9004, Abha (Saudi Arabia); AL-AZHAR University, Faculty of Science, Physics Department, Nasr City, Cairo (Egypt); AlFaify, S. [King Khalid University, Faculty of Science, Physics Department, P.O. Box 9004, Abha (Saudi Arabia)

    2013-09-15

    Assuming an effective mass approximation and using Bastard's boundary conditions, a simple method for simultaneous determination of the energy levels forming the sub-band structure and the transmissions coefficient of non-symmetrical, non-periodical potential semiconducting heterostructure is being proposed. The method can be applied on a multilayer system with varying thickness and effective mass of the layers, and with potential that is neither periodical nor symmetrical. To illustrate the feasibility of the proposed method, cases of symmetrical rectangular triple-barrier structure with constant effective mass, multi-barrier semiconductor heterostructure (nine barriers–eight-wells), and monomer height barrier superlattices (300 barriers) systems have been examined. Findings show very good agreements with previously published results obtained by different methods on similar systems. The proposed method was found to be useful for any number of semiconducting layers arranged in any random way making it more realistic, simple, and applicable to superlattice analysis and for devices design.

  2. Simultaneous determination of water-soluble vitamins in selected food matrices by liquid chromatography/electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Gentili, Alessandra; Caretti, Fulvia; D'Ascenzo, Giuseppe; Marchese, Stefano; Perret, Daniela; Di Corcia, Daniele; Rocca, Lucia Mainero

    2008-07-01

    A rapid, simple and sensitive method based on liquid chromatography/tandem mass spectrometry (LC/MS/MS) with an electrospray ionization (ESI) source for the simultaneous analysis of fourteen water-soluble vitamins (B1, B2, two B3 vitamers, B5, five B6 vitamers, B8, B9, B12 and C) in various food matrices, i.e. maize flour, green and golden kiwi and tomato pulp, is presented here. Analytes were separated by ion-suppression reversed-phase liquid chromatography in less than 10 min and detected in positive ion mode. Sensitivity and specificity of this method allowed two important results to be achieved: (i) limits of detection of the analytes at ng g(-1) levels (except for vitamin C); (ii) development of a rapid sample treatment that minimizes analyte exposition to light, air and heat, eliminating any step of extract concentration. Analyte recovery depended on the type of matrix. In particular, recovery of the analytes in maize flour was > or =70%, with the exception of vitamin C, pyridoxal-5'-phosphate and vitamin B9 (ca 40%); with tomato pulp, recovery was > or =64%, except for vitamin C (41%); with kiwi, recovery was > or =73%, except for nicotinamide (ca. 30%).

  3. Simultaneous determination of vasicine and vasicinone by High-performance liquid chromatography in roots of eight Sida species.

    Science.gov (United States)

    Subramanya, M D; Pai, Sandeep R; Ankad, Gireesh M; Hegde, Harsha V; Roy, Subarna; Hoti, S L

    2016-01-01

    Sida L. is a medicinally important genus widely used in conventional systems of medicine in India. The present study aims toward simultaneous determination of two bioactive compounds vasicine and vasicinone in root extracts of eight Sida spp. from Western Ghats, India. Determination of vasicine and vasicinone was undertaken in methanolic root extracts (10% w/v) of Sida acuta , Sida cordata , Sida cordifolia , Sida rhombifolia , Sida spinosa , Sida indica , Sida retusa and Sida mysorensis by high performance liquid chromatography (HPLC) method. The standards were prepared with the concentration of mg/mL. Data were expressed as mean values of three reading and relative standard deviations. The separation was achieved on a Waters, Nova-Pack, C18 (250 mm × 4.6 mm, 5 μ) column, with acetonitrile - 0.1 M phosphate buffer-glacial acetic acid (15: 85: 1, v/v/v) as solvent system at a flow-rate of 1.0 mL/min. The effluent was monitored using ultraviolet detection at a wavelength of 300 nm. Both calibration curves of standard showed good linear regression ( R 2 > 0.994). The limit of detection and the limit of quantification for vasicine was 0.110 and 0.333 μg/mL and for vasicinone was 0.059 and 0.179 μg/mL respectively. The vasicine content was highest in S. cordifolia (9.891 ± 0.495 μg/100 mg) and vasicinone content was rich in S. cordata (33.013 ± 1.651 μg/100 mg.) The content of vasicinone was higher than vasicine. HPLC method provides simple, accurate, and reproducible quantitative analysis for simultaneous determination of vasicine and vasicinone. Among the selected Sida species, S. cordifolia and S. cordata were found to be rich in the vasicine and vasicinone contents, respectively.

  4. Simultaneous determination of free and total glycerol in biodiesel by capillary electrophoresis using multiple short-end injection.

    Science.gov (United States)

    Spudeit, Daniel Alfonso; Piovezan, Marcel; Dolzan, Maressa D; Vistuba, Jacqueline Pereira; Azevedo, Mônia Stremel; Vitali, Luciano; Leal Oliveira, Marcone Augusto; Oliveira Costa, Ana Carolina; Micke, Gustavo Amadeu

    2013-12-01

    A rapid method for the simultaneous determination of free glycerol (FG) and total glycerol (TG) in biodiesel by CE using a short-end multiple injection (SE/MI) configuration system is described. The sample preparation for FG involves the extraction of glycerol with water and for TG a saponification reaction is carried out followed by extraction as in the case of FG. The glycerol extracted in both cases is submitted to periodate oxidation and the iodate ions formed are measured on a CE-SE/MI system. The relevance of this study lies in the fact that no analytical procedure has been previously reported for the determination of TG (or of FG and TG simultaneously) by CE. The optimum conditions for the saponification/extraction process were 1.25% KOH and 25°C, with a time of only 5 min, and biodiesel mass in the range of 50.0-200.0 mg can be used. Multiple injections were performed hydrodynamically with negative pressure as follows: 50 mbar/3s (FG sample); 50 mbar/6s (electrolyte spacer); 50 mbar/3s (TG sample). The linear range obtained was 1.55-46.5 mg/L with R(2) > 0.99. The LOD and LOQ were 0.16 mg/L and 0.47 mg/L, respectively for TG. The method provides acceptable throughput for application in quality control and monitoring biodiesel synthesis process. In addition, it offers simple sample preparation (saponification process), it can be applied to a variety biodiesel samples (soybean, castor, and waste cooking oils) and it can be used for the determination of two key parameters related to the biodiesel quality with a fast separation (less than 30 s) using an optimized CE-SE/MI system. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. A nanosilver-based spectrophotometry method for sensitive determination of tartrazine in food samples.

    Science.gov (United States)

    Sahraei, R; Farmany, A; Mortazavi, S S

    2013-06-01

    A new method is reported for sensitive determination of tartrazine in the food samples. The method is based on the catalytic effect of silver nanoparticle (AgNPs) on the oxidation reaction of tartrazine by potassium iodate in the acetate buffer medium. The reaction is followed spectrophotometrically by measuring the change in absorbance (ΔA) at 420 nm using a fixed time method (70 s). The reaction variables were optimised in order to achieve the highest sensitivity. The thirty six criterion detection limit was 0.3 ng/mL, and the relative standard deviation for ten replicate measurements of 30 ng/mL of tartrazine was 0.98% (n=10). The method was successfully applied to the determination of tartrazine in lemon, and papaya-flavoured gelatin, candy, and in fruit syrup. Copyright © 2012 Elsevier Ltd. All rights reserved.

  6. Visual Contrast Sensitivity in Early-Stage Parkinson's Disease.

    Science.gov (United States)

    Ming, Wendy; Palidis, Dimitrios J; Spering, Miriam; McKeown, Martin J

    2016-10-01

    Visual impairments are frequent in Parkinson's disease (PD) and impact normal functioning in daily activities. Visual contrast sensitivity is a powerful nonmotor sign for discriminating PD patients from controls. However, it is usually assessed with static visual stimuli. Here we examined the interaction between perception and eye movements in static and dynamic contrast sensitivity tasks in a cohort of mildly impaired, early-stage PD patients. Patients (n = 13) and healthy age-matched controls (n = 12) viewed stimuli of various spatial frequencies (0-8 cyc/deg) and speeds (0°/s, 10°/s, 30°/s) on a computer monitor. Detection thresholds were determined by asking participants to adjust luminance contrast until they could just barely see the stimulus. Eye position was recorded with a video-based eye tracker. Patients' static contrast sensitivity was impaired in the intermediate spatial-frequency range and this impairment correlated with fixational instability. However, dynamic contrast sensitivity and patients' smooth pursuit were relatively normal. An independent component analysis revealed contrast sensitivity profiles differentiating patients and controls. Our study simultaneously assesses perceptual contrast sensitivity and eye movements in PD, revealing a possible link between fixational instability and perceptual deficits. Spatiotemporal contrast sensitivity profiles may represent an easily measurable metric as a component of a broader combined biometric for nonmotor features observed in PD.

  7. Simultaneous quantification of seven hippocampal neurotransmitters in depression mice by LC-MS/MS.

    Science.gov (United States)

    Huang, Fei; Li, Jia; Shi, Hai-Lian; Wang, Ting-ting; Muhtar, Wahaf; Du, Min; Zhang, Bei-bei; Wu, Hui; Yang, Li; Hu, Zhi-bi; Wu, Xiao-jun

    2014-05-30

    There is no method available to simultaneously detect GABA, Glu, Epi, NE, DA, 5-HT and 5-HIAA in mouse hippocampus. A rapid and sensitive LC-MS/MS method has been developed for simultaneously measuring seven neurotransmitters in mouse hippocampus. The analytes were detected in positive mode with multiple reaction monitoring (MRM) and the procedure was completed in less than 9min. This method exhibited excellent linearity for all of the analytes with regression coefficients higher than 0.99, and showed good intra- and inter-day precisions (RSDneurotransmitters in a mouse depression model induced by successive methylprednisolone injections. The results indicated that this depression model was closely associated with the decreased level of Epi (p=0.002) and elevated ratio of 5-HIAA/5-HT (p=0.01), which has never been reported elsewhere. Compared with previous methods, current approach is more convenient without any pre-column derivatization of the analytes but enhances detectability with incremental neurotransmitter profile and shortens detection time. This work represents the first accurate simultaneous determination of seven neurotransmitters in the mouse depression model induced by methylprednisolone. The reliable method will benefit the research of neurological diseases with the altered neurotransmitter profile in brain. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. The application of the inductively coupled plasma system to the simultaneous determination of precious metals

    International Nuclear Information System (INIS)

    Watson, A.E.; Russell, G.M.; Middleton, H.R.; Davenport, F.F.

    1983-01-01

    This report describes the development of a spectrochemical technique using excitation by an inducticely coupled plasma (ICP) source for the simultaneous determination of the precious metals (defined here as gold, silver, and all the platinum-group metals except osmium) in a wide variety of samples from a plant for the extraction and refining of platinum metal. The limits of detection for the analytes were determined in various acid and salt media and, under the conditions used, ranged from 20 to 100ng/l. The analytes were determined in the presence of a thousandfold excess of each of the other precious metals used as a matrix element. Some severe interferences were noted but were ascribed to spectral-line overlap or to contamination of the matrix material. Various dissolution techniques, based upon standard procedures applied in the precious-metals industry, were used, depending on the particular type of material treated. The spectrometer was calibrated by the use of solutions containing the analytes, sodium chloride, and acid, with scandium as the internal standard. The accuracy and precision of the technique, established by the analysis of many samples of each type, were found to be satisfactory when close attention was paid to detail in the preparation of the analytical solution. The relative standard deviation of the method ranges from 0,005 to 0,05, depending on the element being determined

  9. A binderless, covalently bulk modified electrochemical sensor: Application to simultaneous determination of lead and cadmium at trace level

    Energy Technology Data Exchange (ETDEWEB)

    Gunigollahalli Kempegowda, Raghu [Department of Studies in Chemistry, Bangalore University, Central College Campus, Bangalore 560001 (India); Malingappa, Pandurangappa, E-mail: mprangachem@gmail.com [Department of Studies in Chemistry, Bangalore University, Central College Campus, Bangalore 560001 (India)

    2012-05-30

    Highlights: Black-Right-Pointing-Pointer Proposed sensor is a new type of binderless covalent bulk modified electrode. Black-Right-Pointing-Pointer Surface can be easily renewed by simple mechanical polishing using emery sheets. Black-Right-Pointing-Pointer Free from modifier leaching during electrochemical measurements. Black-Right-Pointing-Pointer Provides long term storage stability with good reproducibility. Black-Right-Pointing-Pointer Nanomolar level detection limit achieved with selectivity. - Abstract: A new type of covalent binderless bulk modified electrode has been fabricated and used in the simultaneous determination of lead and cadmium ions at nanomolar level. The modification of graphitic carbon with 4-amino salicylic acid was carried out under microwave irradiation through the amide bond formation. The electrochemical behavior of the fabricated electrode has been carried out to decipher the interacting ability of the functional moieties present on the modifier molecules toward the simultaneous determination of Pb{sup 2+} and Cd{sup 2+} ions using cyclic and differential pulse anodic stripping voltammetry. The possible mode of interaction of functional groups with metal ions is proposed based on the pKa values of the modifier functionalities present on the surface of graphitic carbon particles. The analytical utility of the proposed sensor has been validated by measuring the lead and cadmium content from pretreated waste water samples of lead acid batteries.

  10. Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine

    International Nuclear Information System (INIS)

    Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming

    2013-01-01

    Graphical abstract: -- Highlights: •A green and facile approach for synthesis of β-CD-PDDA-Gr at room temperature. •We present the β-CD-PDDA-Gr modified GC-RDE for simultaneous detection of SY and TT. •SY and TT's electrooxidations are both the one-electron-one-proton-transfer process. •Diffusion coefficients and standard rate constants of SY and TT were discussed. -- Abstract: We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant k b , were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0 × 10 −8 to 2.0 × 10 −5 mol L −1 , with a low limit of detection (LOD) of 1.25 × 10 −8 mol L −1 for SY and 1.43 × 10 −8 mol L −1 for TT (S N −1 = 3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant differences were found. By the treatment of the

  11. Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine

    Energy Technology Data Exchange (ETDEWEB)

    Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming, E-mail: wangcm@lzu.edu.cn

    2013-05-24

    Graphical abstract: -- Highlights: •A green and facile approach for synthesis of β-CD-PDDA-Gr at room temperature. •We present the β-CD-PDDA-Gr modified GC-RDE for simultaneous detection of SY and TT. •SY and TT's electrooxidations are both the one-electron-one-proton-transfer process. •Diffusion coefficients and standard rate constants of SY and TT were discussed. -- Abstract: We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant k{sub b}, were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0 × 10{sup −8} to 2.0 × 10{sup −5} mol L{sup −1}, with a low limit of detection (LOD) of 1.25 × 10{sup −8} mol L{sup −1} for SY and 1.43 × 10{sup −8} mol L{sup −1} for TT (S N{sup −1} = 3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant

  12. Photo-polarimetric sensitivities to layering and mixing of absorbing aerosols

    Directory of Open Access Journals (Sweden)

    O. V. Kalashnikova

    2011-09-01

    Full Text Available We investigate to what extent multi-angle polarimetric measurements are sensitive to vertical mixing/layering of absorbing aerosols, adopting calibration uncertainty of 1.5% in intensity and 0.5% in the degree of linear polarization of Multiangle Spectro-Polarimetric Imager (MSPI. Employing both deterministic and Monte Carlo radiative transfer codes with polarization, we conduct modeling experiments to determine how the measured Stokes vector elements are affected at UV and short visible wavelengths by the vertical distribution, mixing and layering of smoke and dust aerosols for variety of microphysical parameters. We find that multi-angular polarimetry holds the potential to infer dust-layer heights and thicknesses at blue visible channel due to its lesser sensitivity to changes in dust coarse mode optical properties, but higher sensitivity to the dust vertical profiles. Our studies quantify requirements for obtaining simultaneous information on aerosol layer height and absorption under MSPI measurement uncertainties.

  13. Differential antibiotic sensitivity determined by the large ribosomal subunit in thermophilic archaea.

    OpenAIRE

    Ruggero, D; Londei, P

    1996-01-01

    Hybrid ribosomes obtained by mixing the ribosomal subunits of the extremely thermophilic archaea Sulfolobus solfataricus and Desulfurococcus mobilis were tested for their sensitivity to selected antibiotics. It is shown that structural differences in the large ribosomal subunits determine qualitatively and quantitatively the patterns of response to alpha-sarcin and paromomycin in these species.

  14. Simultaneous Determination of Ten Constituents in Chaiqin Qingning Capsule by High-performance Liquid Chromatography Coupled with Triple-quadrupole Mass Spectrometry.

    Science.gov (United States)

    Li, Ting Yu; Huo, Xiao Kui; Zheng, Lu; Wang, Chao; Cong, Hai Jian; Xiang, Ting; Zhang, Lin; Zhang, Bao Jing; Huang, Shan Shan; Wu, Bin; Li, Xin Yu

    2017-01-01

    Chaiqin Qingning Capsule (CQQNC) was a prescription of Traditional Chinese Medicine with the effects of clearing away heat and removing toxin, harmonizing the exterior and interior, it was widely used in Asian, for example, China and Japan, different batches of the raws materials and different processing time may be the vital factor which raised a challenge to control the quality of the CQQNC. In this experiment, a high-performance liquid chromatography-mass spectrometry/MS (HPLC-MS/MS) method was developed to simultaneously determine ten bioactive components for the quality control of CQQNC. Chromatographic separation was achieved using an XBridge BEH C18 column (150 mm × 4.6 mm, 2.5 μm) with a mobile phase composed of 10 mm aqueous ammonium acetate and acetonitrile using a gradient elution in 20 min. This study was conducted by multiple reaction monitoring mode through electrospray ionization resource with a negative ionization mode. The established method was validated with good performance of precision, accuracy, stability, and reproducibility and was utilized to simultaneously quantify ten constituents of CQQNC obtained from seven different batches. It is the first time to report the rapid and simultaneous analysis of the ten compounds in CQQNC by HPLC-MS/MS and apply to determine 10 constituents in 7 batches of CQQNC bought from drug store in china. This method could be considered as good quality criteria to control the quality of CQQNC. In this paper, a simple, specific, and rapid high-performance liquid chromatogram coupled with triple-quadrupole mass spectrometry method for simultaneous quantification of ten constituents in Chaiqin Qingning Capsule has been developed for the first time. This method could be considered as good quality criteria to control the quality of CQQNC. Abbreviations used: CHM: Chinese herbal medicine; TCM: Traditional Chinese Medicine; CQQNC: Triple-quadrupole mass spectrometry Chaiqin Qingning Capsules; HPLC-MS/MS: High liquid

  15. Simultaneous Determination of Ten Constituents in Chaiqin Qingning Capsule by High-performance Liquid Chromatography Coupled with Triple-quadrupole Mass Spectrometry

    Science.gov (United States)

    Li, Ting Yu; Huo, Xiao Kui; Zheng, Lu; Wang, Chao; Cong, Hai Jian; Xiang, Ting; Zhang, Lin; Zhang, Bao Jing; Huang, Shan Shan; Wu, Bin; Li, Xin Yu

    2017-01-01

    Background: Chaiqin Qingning Capsule (CQQNC) was a prescription of Traditional Chinese Medicine with the effects of clearing away heat and removing toxin, harmonizing the exterior and interior, it was widely used in Asian, for example, China and Japan, different batches of the raws materials and different processing time may be the vital factor which raised a challenge to control the quality of the CQQNC. Experimental Methods: In this experiment, a high-performance liquid chromatography-mass spectrometry/MS (HPLC-MS/MS) method was developed to simultaneously determine ten bioactive components for the quality control of CQQNC. Chromatographic separation was achieved using an XBridge BEH C18 column (150 mm × 4.6 mm, 2.5 μm) with a mobile phase composed of 10 mm aqueous ammonium acetate and acetonitrile using a gradient elution in 20 min. This study was conducted by multiple reaction monitoring mode through electrospray ionization resource with a negative ionization mode. Results: The established method was validated with good performance of precision, accuracy, stability, and reproducibility and was utilized to simultaneously quantify ten constituents of CQQNC obtained from seven different batches. Conclusion: It is the first time to report the rapid and simultaneous analysis of the ten compounds in CQQNC by HPLC-MS/MS and apply to determine 10 constituents in 7 batches of CQQNC bought from drug store in china. This method could be considered as good quality criteria to control the quality of CQQNC. SUMMARY In this paper, a simple, specific, and rapid high-performance liquid chromatogram coupled with triple-quadrupole mass spectrometry method for simultaneous quantification of ten constituents in Chaiqin Qingning Capsule has been developed for the first time. This method could be considered as good quality criteria to control the quality of CQQNC. Abbreviations used: CHM: Chinese herbal medicine; TCM: Traditional Chinese Medicine; CQQNC: Triple-quadrupole mass

  16. H-Point Standard Addition Method for Simultaneous Determination of Eosin and Erytrosine

    Directory of Open Access Journals (Sweden)

    Amandeep Kaur

    2011-01-01

    Full Text Available A new, simple, sensitive and selective H-point standard addition method (HPSAM has been developed for resolving binary mixture of food colorants eosin and erythrosine, which show overlapped spectra. The method is based on the complexation of food dyes eosin and erythrosine with Fe(III complexing reagent at pH 5.5 and solubilizing complexes in triton x-100 micellar media. Absorbances at the two pairs of wavelengths, 540 and 550 nm (when eosin acts as analyte or 518 and 542 nm (when erythrosine act as analyte were monitored. This method has satisfactorily been applied for the determination of eosin and erythrosine dyes in synthetic mixtures and commercial products.

  17. Ultrasound-assisted extraction method for the simultaneous determination of emerging contaminants in freshwater sediments.

    Science.gov (United States)

    de Sousa, Diana Nara Ribeiro; Grosseli, Guilherme Martins; Mozeto, Antonio Aparecido; Carneiro, Renato Lajarim; Fadini, Pedro Sergio

    2015-10-01

    Sediments are the fate of several emerging organic contaminants, such as pharmaceuticals, personal care products and hormones, and therefore an important subject in environmental monitoring studies. In the present work, a simple and sensitive method was developed, validated and applied for the simultaneous extraction of atenolol, caffeine, carbamazepine, diclofenac, ibuprofen, naproxen, propranolol, triclosan, estrone, 17-β-estradiol and 17-α-ethinylestradiol using ultrasound-assisted extraction from freshwater sediment samples followed by solid-phase extraction clean-up and liquid chromatography with tandem mass spectrometry detection. The solvent type and extraction pH were evaluated to obtain the highest recoveries of the compounds. The best method shows absolute recoveries between 54.0 and 94.4% at 50 ng/g concentration. The method exhibits good precision with relative standard deviation ranging from 1.0-16%. The detection and quantification limits ranged from 0.006-0.067 and 0.016-0.336 ng/g, respectively. The developed method was successfully applied to freshwater sediment samples collected from different sites in Jundiaí River basin of São Paulo State, Brazil. The compounds atenolol, caffeine, propranolol and triclosan were detected in all the sampling sites with concentrations of 13.8, 41.0, 28.5 and 176 ng/g, respectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. PET Imaging Stability Measurements During Simultaneous Pulsing of Aggressive MR Sequences on the SIGNA PET/MR System.

    Science.gov (United States)

    Deller, Timothy W; Khalighi, Mohammad Mehdi; Jansen, Floris P; Glover, Gary H

    2018-01-01

    The recent introduction of simultaneous whole-body PET/MR scanners has enabled new research taking advantage of the complementary information obtainable with PET and MRI. One such application is kinetic modeling, which requires high levels of PET quantitative stability. To accomplish the required PET stability levels, the PET subsystem must be sufficiently isolated from the effects of MR activity. Performance measurements have previously been published, demonstrating sufficient PET stability in the presence of MR pulsing for typical clinical use; however, PET stability during radiofrequency (RF)-intensive and gradient-intensive sequences has not previously been evaluated for a clinical whole-body scanner. In this work, PET stability of the GE SIGNA PET/MR was examined during simultaneous scanning of aggressive MR pulse sequences. Methods: PET performance tests were acquired with MR idle and during simultaneous MR pulsing. Recent system improvements mitigating RF interference and gain variation were used. A fast recovery fast spin echo MR sequence was selected for high RF power, and an echo planar imaging sequence was selected for its high heat-inducing gradients. Measurements were performed to determine PET stability under varying MR conditions using the following metrics: sensitivity, scatter fraction, contrast recovery, uniformity, count rate performance, and image quantitation. A final PET quantitative stability assessment for simultaneous PET scanning during functional MRI studies was performed with a spiral in-and-out gradient echo sequence. Results: Quantitation stability of a 68 Ge flood phantom was demonstrated within 0.34%. Normalized sensitivity was stable during simultaneous scanning within 0.3%. Scatter fraction measured with a 68 Ge line source in the scatter phantom was stable within the range of 40.4%-40.6%. Contrast recovery and uniformity were comparable for PET images acquired simultaneously with multiple MR conditions. Peak noise equivalent count

  19. The comparison of partial least squares and principal component regression in simultaneous spectrophotometric determination of ascorbic acid, dopamine and uric acid in real samples

    Directory of Open Access Journals (Sweden)

    Habiboallah Khajehsharifi

    2017-05-01

    Full Text Available Partial least squares (PLS1 and principal component regression (PCR are two multivariate calibration methods that allow simultaneous determination of several analytes in spite of their overlapping spectra. In this research, a spectrophotometric method using PLS1 is proposed for the simultaneous determination of ascorbic acid (AA, dopamine (DA and uric acid (UA. The linear concentration ranges for AA, DA and UA were 1.76–47.55, 0.57–22.76 and 1.68–28.58 (in μg mL−1, respectively. However, PLS1 and PCR were applied to design calibration set based on absorption spectra in the 250–320 nm range for 36 different mixtures of AA, DA and UA, in all cases, the PLS1 calibration method showed more quantitative prediction ability than PCR method. Cross validation method was used to select the optimum number of principal components (NPC. The NPC for AA, DA and UA was found to be 4 by PLS1 and 5, 12, 8 by PCR. Prediction error sum of squares (PRESS of AA, DA and UA were 1.2461, 1.1144, 2.3104 for PLS1 and 11.0563, 1.3819, 4.0956 for PCR, respectively. Satisfactory results were achieved for the simultaneous determination of AA, DA and UA in some real samples such as human urine, serum and pharmaceutical formulations.

  20. Simultaneous determination of 3-monochloropropane-1,2-diol and acrylamide in food by gas chromatography-triple quadrupole mass spectrometry with coupled column separation.

    Science.gov (United States)

    Xu, Xiao-min; He, Hua-li; Zhu, Yan; Feng, Liang; Ying, Ying; Huang, Bai-fen; Shen, Hai-tao; Han, Jian-long; Ren, Yi-ping

    2013-01-14

    Both 3-monochloropropane-1,2-diol (3-MCPD) and acrylamide are contaminants found in heat-processed foods and their related products. A quantitative method was developed for the simultaneous determination of both contaminants in food by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The analytes were purified and extracted by the matrix solid-phase dispersion extraction (MSPDE) technique with Extrelut NT. A coupled column (a 3 m Innowax combined with a 30 m DB-5 ms) was developed to separate both compounds efficiently without derivatization. Triple quadrupole mass spectrometry in multiple reaction monitoring mode (MRM) was applied to suppress matrix interference and obtain good sensitivity in the determination of both analytes. The limit of detection (LOD) in the sample matrix was 5 μg kg(-1) for 3-MCPD or acrylamide. The average recoveries for 3-MCPD and acrylamide in different food matrices were 90.5-107% and 81.9-95.7%, respectively, with the intraday relative standard deviations (RSDs) of 5.6-13.5% and 5.3-13.4%, respectively. The interday RSDs were 6.1-12.6% for 3-MCPD and were 5.0-12.8% for acrylamide. Both contaminants were found in samples of bread, fried chips, fried instant noodles, soy sauce, and instant noodle flavoring. Neither 3-MCPD nor acrylamide was detected in the samples of dairy products (solid or liquid samples) and non-fried instant noodles. Copyright © 2012 Elsevier B.V. All rights reserved.