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Sample records for chromatography high pressure liquid

  1. Method transfer from high-pressure liquid chromatography to ultra-high-pressure liquid chromatography. II. Temperature and pressure effects.

    Science.gov (United States)

    Åsberg, Dennis; Samuelsson, Jörgen; Leśko, Marek; Cavazzini, Alberto; Kaczmarski, Krzysztof; Fornstedt, Torgny

    2015-07-03

    The importance of the generated temperature and pressure gradients in ultra-high-pressure liquid chromatography (UHPLC) are investigated and compared to high-pressure liquid chromatography (HPLC). The drug Omeprazole, together with three other model compounds (with different chemical characteristics, namely uncharged, positively and negatively charged) were used. Calculations of the complete temperature profile in the column at UHPLC conditions showed, in our experiments, a temperature difference between the inlet and outlet of 16 °C and a difference of 2 °C between the column center and the wall. Through van't Hoff plots, this information was used to single out the decrease in retention factor (k) solely due to the temperature gradient. The uncharged solute was least affected by temperature with a decrease in k of about 5% while for charged solutes the effect was more pronounced, with k decreases up to 14%. A pressure increase of 500 bar gave roughly 5% increase in k for the uncharged solute, while omeprazole and the other two charged solutes gave about 25, 20 and 15% increases in k, respectively. The stochastic model of chromatography was applied to estimate the dependence of the average number of adsorption/desorption events (n) and the average time spent by a molecule in the stationary phase (τs) on temperature and pressure on peak shape for the tailing, basic solute. Increasing the temperature yielded an increase in n and decrease in τs which resulted in less skew at high temperatures. With increasing pressure, the stochastic modeling gave interesting results for the basic solute showing that the skew of the peak increased with pressure. The conclusion is that pressure effects are more pronounced for both retention and peak shape than the temperature effects for the polar or charged compounds in our study.

  2. 21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to...

  3. HPLC separation and GC-MS identification of the polar components of coal liquids. [High pressure liquid chromatography, gas chromatography-mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Satoh, M.; Tanabe, K.; Uchino, H.; Yokoyama, S.; Sanada, Y.

    1984-01-01

    The polar components in the 200-400 C fraction of Akabira coal liquids were separated by high pressure liquid chromatography using an amine-based column. By varying the CHCl/sub 3/ concentration in the solvent, basic, neutral and acid fractions were obtained. These were then investigated separately using infrared spectroscopy, flame ionization detection-gas chromatography and gas chromatography-mass spectroscopy. The basic fraction contained alkyltetrahydroquinolines, the neutral fraction, alkylphenols and alkylcarbazoles; and the acid fraction, alkylphenols. 15 references.

  4. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography

    NARCIS (Netherlands)

    Uliyanchenko, E.; van der Wal, S.; Schoenmakers, P.J.

    2011-01-01

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles an

  5. Benzoin Condensation: Monitoring a Chemical Reaction by High-Pressure Liquid Chromatography

    Science.gov (United States)

    Bhattacharya, Apurba; Purohit, Vikram C.; Bellar, Nicholas R.

    2004-01-01

    High-pressure liquid chromatography (HPLC) is the preferred method of separating a variety of materials in complex mixtures such as pharmaceuticals, polymers, soils, food products and biological fluids and is also considered to be a powerful analytical tool in both academia and industry. The use of HPLC analysis as a means of monitoring and…

  6. Evaluation between ultrahigh pressure liquid chromatography and high-performance liquid chromatography analytical methods for characterizing natural dyestuffs.

    Science.gov (United States)

    Serrano, Ana; van Bommel, Maarten; Hallett, Jessica

    2013-11-29

    An evaluation was undertaken of ultrahigh pressure liquid chromatography (UHPLC) in comparison to high-performance liquid chromatography (HPLC) for characterizing natural dyes in cultural heritage objects. A new UHPLC method was optimized by testing several analytical parameters adapted from prior UHPLC studies developed in diverse fields of research. Different gradient elution programs were tested on seven UHPLC columns with different dimensions and stationary phase compositions by applying several mobile phases, flow rates, temperatures, and runtimes. The UHPLC method successfully provided more improved data than that achieved by the HPLC method. Indeed, even though carminic acid has shown circa 146% higher resolution with HPLC, UHPLC resulted in an increase of 41-61% resolution and a decrease of 91-422% limit of detection, depending on the dye compound. The optimized method was subsequently assigned to analyse 59 natural reference materials, in which 85 different components were ascribed with different physicochemical properties, in order to create a spectral database for future characterization of dyes in cultural heritage objects. The majority of these reference samples could be successfully distinguished with one single method through the examination of these compounds' retention times and their spectra acquired with a photodiode array detector. These results demonstrate that UHPLC analyses are extremely valuable for the acquisition of more precise chromatographic information concerning natural dyes with complex mixtures of different and/or closely related physicochemical properties, essential for distinguishing similar species of plants and animals used to colour cultural heritage objects.

  7. High Performance Liquid Chromatography

    Science.gov (United States)

    Talcott, Stephen

    High performance liquid chromatography (HPLC) has many applications in food chemistry. Food components that have been analyzed with HPLC include organic acids, vitamins, amino acids, sugars, nitrosamines, certain pesticides, metabolites, fatty acids, aflatoxins, pigments, and certain food additives. Unlike gas chromatography, it is not necessary for the compound being analyzed to be volatile. It is necessary, however, for the compounds to have some solubility in the mobile phase. It is important that the solubilized samples for injection be free from all particulate matter, so centrifugation and filtration are common procedures. Also, solid-phase extraction is used commonly in sample preparation to remove interfering compounds from the sample matrix prior to HPLC analysis.

  8. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography.

    Science.gov (United States)

    Uliyanchenko, Elena; van der Wal, Sjoerd; Schoenmakers, Peter J

    2011-09-28

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles and narrow bore tubing in combination with high pressures generate significant shear and extensional forces in UHPLC systems, which may affect polymer chains. At high stress conditions flexible macromolecules may become extended and eventually the chemical bonds in the molecules can break. Deformation and degradation of macromolecules will affect the peak retention and the peak shape in the chromatogram, which may cause errors in the obtained results (e.g. the calculated molecular-weight distributions). In the present work we explored the limitations of UHPLC for the analysis of polymers. Degradation and deformation of macromolecules were studied by collecting and re-injecting polymer peaks and by off-line two-dimensional liquid chromatography. Polystyrene standards with molecular weight of 4 MDa and larger were found to degrade at UHPLC conditions. However, for most polymers degradation could be avoided by using low linear velocities. No degradation of 3-MDa PS (and smaller) was observed at linear velocities up to 7 mm/s. The column frits were implicated as the main sources of polymer degradation. The extent of degradation was found to depend on the type of the column and on the column history. At high flow rates degradation was observed without a column being installed. We demonstrated that polymer deformation preceded degradation. Stretched polymers eluted from the column in slalom chromatography mode (elution order opposite to that in SEC or HDC). Under certain conditions we observed co-elution of large and small PS molecules though a convolution of slalom chromatography and hydrodynamic chromatography.

  9. Muramic Acid Measurements for Bacterial Investigations in Marine Environments by High-Pressure Liquid Chromatography

    Science.gov (United States)

    Mimura, Toru; Romano, Jean-Claude

    1985-01-01

    Muramic acid, a constituent of procaryotic cell walls, was assayed by high-pressure liquid chromatography in samples from several marine environments (water column, surface microlayer, and sediment) and a bacterial culture. It is used as a microbial biomass indicator. The method gave a good separation of muramic acid from interfering compounds with satisfactory reproducibility. A pseudomonad culture had a muramic acid content of 4.7 × 10−10 to 5.3 × 10−10 μg per cell during growth. In natural water samples, highly significant relationships were found between muramic acid concentrations and bacterial numbers for populations of 108 to 1011 cells per liter. The muramic acid content in natural marine water decreased from 5.3 × 10−10 to 1.6 × 10−10 μg per cell with increasing depth. In coastal sediments exposed to sewage pollution, concentrations of muramic acid, ATP, organic carbon, and total amino acids displayed a parallel decrease with increasing distance from the sewage outlet. Advantages of muramic acid measurement by high-pressure liquid chromatography are its high sensitivity and reduction of preparation steps, allowing a short time analysis. PMID:16346848

  10. Adaptation of a High-Pressure Liquid Chromatography System for the Measurement of Viscosity

    Directory of Open Access Journals (Sweden)

    Sonia Gregory

    2014-03-01

    Full Text Available The state-of-the-art instruments for the determination of viscosity of liquids typically require a significant amount of sample, and have relatively low throughput due to manual and sequential measurements. In this study, it was demonstrated that the pressure generated by the flow of viscous fluids through a capillary could be precisely measured employing high-pressure liquid chromatography systems (HPLC using glycerol solutions of moderate viscosity as a mobile phase, and correlated to the dynamic (absolute viscosity. The parameters allowing calculation of the viscosity of glycerol calibration standards as a function of temperature were established. The measurements were made with volumes as small as 10 μL, and the use of an autosampler permitted unattended analysis of a large number samples. The method appears to be particularly well suited for the development of viscous formulations of therapeutic, protein-based macromolecules, where the amount sample is typically limited and relatively wide ranges of conditions are considered in the optimization process. The utility of the methods was illustrated by application to the development of concentrated inactivated virus vaccines.

  11. Analysis of penicillin N ring expansion activity from Streptomyces clavuligerus by ion-pair high-pressure liquid chromatography.

    OpenAIRE

    JENSEN, S. E.; Westlake, D W; Wolfe, S.

    1983-01-01

    An ion-pair, reversed-phase, high-pressure liquid chromatographic method for the analysis of penicillin N ring expansion activity has been developed which allows simultaneous measurement of both substrate and product. The high-pressure liquid chromatography conditions were as follows: stationary phase, C18; flow rate, 2 ml/min; detection, 220 nm. The stationary phase was preconditioned with 4.5 mM tetrabutylammonium bromide in 0.05 M KH2PO4 (pH 4.0)-methanol (85:15, vol/vol) and then equilibr...

  12. Assessment of radiochemical purity of [{sup 18}F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z., E-mail: radiofarmacoscdtn@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Producao de Radiofarmacos

    2011-07-01

    The quality control of [{sup 18}F]fludeoxyglucose ({sup 18}FDG) has received attention due to its increasing clinical use. Although the quality requirements of {sup 18}FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of {sup 18}FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. {sup 18}FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of {sup 18}FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of {sup 18}FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of {sup 18}FDG, considering operational conditions of our laboratory. (author)

  13. Standardization of a fluconazole bioassay and correlation of results with those obtained by high-pressure liquid chromatography.

    OpenAIRE

    Rex, J H; Hanson, L H; Amantea, M A; Stevens, D.A.; BENNETT,J.E.

    1991-01-01

    An improved bioassay for fluconazole was developed. This assay is sensitive in the clinically relevant range (2 to 40 micrograms/ml) and analyzes plasma, serum, and cerebrospinal fluid specimens; bioassay results correlate with results obtained by high-pressure liquid chromatography (HPLC). Bioassay and HPLC analyses of spiked plasma, serum, and cerebrospinal fluid samples (run as unknowns) gave good agreement with expected values. Analysis of specimens from patients gave equivalent results b...

  14. High-Pressure Liquid Chromatography of Irradiated Nuclear Fue - Separation of Neodymium for Burn-up Determination

    DEFF Research Database (Denmark)

    Larsen, N. R.

    1979-01-01

    Neodymium is separated from solutions of spent nuclear fuel by high-pressure liquid chromatography in methanol-nitric acid-water media using an anion-exchange column. Chromatograms obtained by monitoring at 280 nm, illustrate the difficulties especially with the fission product ruthenium in nuclear...... chemistry. Preseparation of the rare earths and trivalent actinides using a di(2-ethylhexyl)phosphoric acid/kieselguhr column is described....

  15. Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

    Science.gov (United States)

    Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

    2016-03-18

    Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs.

  16. Determination of tetracycline antibiotics in fatty food samples by selective pressurized liquid extraction coupled with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Jiao, Zhe; Zhang, Suling; Chen, Hongwei

    2015-01-01

    For the determination of trace residues of tetracycline antibiotics in fatty food samples, selective pressurized liquid extraction coupled with high-performance liquid chromatography and tandem mass spectrometry was applied in this study. Copper(II) isonicotinate was first used as online cleanup adsorbent in the selective pressurized liquid extraction process. The adsorbent to sample ratio, extraction temperature, extraction time, and recycle times, etc. were optimized. The tetracyclines in food samples of pork, chicken meat, and clam meat were detected by liquid chromatography with tandem mass spectrometry. Tetracycline was found at levels of 0.32 and 0.53 μg/g and oxytetracycline was found at 0.14 and 0.21 μg/g in chicken meat and clam meat, respectively, while chlorotetracycline and deoxytetracycline were below the detection limit. The detection limit (S/N = 3) for these four tetracyclines were from 0.2 to 3.3 ng/g, the recoveries were from 75.8 to 110.5%, and relative standard deviations were from 5.5 to 13.6%. Copper(II) isonicotinate showed a higher purification capacity than other cleanup adsorbents for extraction of antibiotics in fatty food and the recovery showed predominance compared with a pressurized liquid extraction method without adsorbent. The study demonstrated that copper(II) isonicotinate would be a promising cleanup adsorbent in pressurized liquid extraction for the analysis of trace organic pollutants in complicated samples.

  17. Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

    Science.gov (United States)

    Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

    2016-08-01

    Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract.

  18. Rapid quantification of cyanamide by ultra-high-pressure liquid chromatography in fertilizer, soil or plant samples.

    Science.gov (United States)

    Nagumo, Yoshifumi; Tanaka, Kazuya; Tewari, Kaushal; Thiraporn, Khwankaew; Tsuchida, Toru; Honma, Toshimitsu; Ohtake, Norikuni; Sueyoshi, Kuni; Takahashi, Yoshihiko; Ohyama, Takuji

    2009-07-17

    A rapid and simple method for determination of cyanamide in fertilizer, soil and plants has been developed. In this method, cyanamide is extracted with 2% acetic acid and the extract separated by centrifugation. It is then purified by passing through a membrane filter. The extract was derivatized with 6-aminoquinolyl-N-hydroxysuccinimidyl-carbamate and the derivatized compound separated by ultra-high-pressure liquid chromatography. It is then detected with a UV detector at 260 nm by the same method as is used for amino acid analysis. The proposed method is fast, simple and cheap and also has good selectivity and sensitivity for the determination of cyanamide in a wide range of biotic and abiotic materials.

  19. Comparative analysis of different plant oils by high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

    Science.gov (United States)

    Jakab, Annamaria; Héberger, Károly; Forgács, Esther

    2002-11-01

    Different vegetable oil samples (almond, avocado, corngerm, grapeseed, linseed, olive, peanut, pumpkin seed, soybean, sunflower, walnut, wheatgerm) were analyzed using high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry. A gradient elution technique was applied using acetone-acetonitrile eluent systems on an ODS column (Purospher, RP-18e, 125 x 4 mm, 5 microm). Identification of triacylglycerols (TAGs) was based on the pseudomolecular ion [M+1]+ and the diacylglycerol fragments. The positional isomers of triacylglycerol were identified from the relative intensities of the [M-RCO2]+ fragments. Linear discriminant analysis (LDA) as a common multivariate mathematical-statistical calculation was successfully used to distinguish the oils based on their TAG composition. LDA showed that 97.6% of the samples were classified correctly.

  20. Preparative Isolation and Purification of Flavone C-Glycosides from the Leaves of Ficus microcarpa L. f by Medium-Pressure Liquid Chromatography, High-Speed Countercurrent Chromatography, and Preparative Liquid Chromatography.

    Science.gov (United States)

    Wang, Xiaohong; Liang, Yong; Zhu, Licai; Xie, Huichun; Li, Hang; He, Junting; Pan, Man; Zhang, Tianyou; Ito, Yoichiro

    2010-01-01

    Combined with medium-pressure liquid chromatography (MPLC) and preparative high-performance liquid chromatography (perp-HPLC), high-speed countercurrent chromatography (HSCCC) was applied for separation and purification of flavone C-glycosides from the crude extract of leaves of Ficus microcarpae L. f. HSCCC separation was performed on a two-phase solvent system composed of methyl tert- butyl ether - ethyl acetate - 1-butanol - acetonitrile - 0.1% aqueous trifluoroacetic acid at a volume ratio of 1:3:1:1:5. Partially resolved peak fractions from HSCCC separation were further purified by preparative HPLC. Four well-separated compounds were obtained and their purities were determined by HPLC. The purities of these peaks were 97.28%, 97.20%, 92.23%, and 98.40%.. These peaks were characterized by ESI-MS(n). According to the reference, they were identified as orientin (peak I), isovitexin-3″-O-glucopyranoside (peak II), isovitexin (peak III), and vitexin (peak IV), yielded 1.2 mg, 4.5 mg, 3.3 mg, and 1.8 mg, respectively.

  1. Quantification of antidepressants and antipsychotics in human serum by precipitation and ultra high pressure liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Hasselstrøm, Jørgen Bo

    2011-01-01

    precipitated with zinc sulphate and methanol containing a stable isotope labelled analog for each analyte. Quantitative analysis was performed by ultra high pressure liquid chromatography combined with a tandem mass spectrometer using a Zorbax SB-C8 column (2.0×50mm; 1.8m) with a mobile phase consisting of 0...... for therapeutic drug monitoring. The method was developed to replace old techniques which applied solid phase extraction and ultra-violet detection. The old methods had reached their limit of capacity regarding the number of samples and co-medicated drugs interfering with the detection. Serum samples were.......1% formic acid in water and methanol, respectively. The total run time of the chromatography was 4 min. Precision and trueness varied from 2.6% to 14.9% and 87.6% to 103.5%, respectively. At the lower limit of quantification, precision was up to 17.9% and trueness varied from 89.5% to 111.5%. A five point...

  2. Quantification aspects of constant pressure (ultra) high pressure liquid chromatography using mass-sensitive detectors with a nebulizing interface.

    Science.gov (United States)

    Verstraeten, M; Broeckhoven, K; Lynen, F; Choikhet, K; Landt, K; Dittmann, M; Witt, K; Sandra, P; Desmet, G

    2013-01-25

    The present contribution investigates the quantitation aspects of mass-sensitive detectors with nebulizing interface (ESI-MSD, ELSD, CAD) in the constant pressure gradient elution mode. In this operation mode, the pressure is controlled and maintained at a set value and the liquid flow rate will vary according to the inverse mobile phase viscosity. As the pressure is continuously kept at the allowable maximum during the entire gradient run, the average liquid flow rate is higher compared to that in the conventional constant flow rate operation mode, thus shortening the analysis time. The following three mass-sensitive detectors were investigated: mass spectrometry detector (MS), evaporative light scattering detector (ELSD) and charged aerosol detector (CAD) and a wide variety of samples (phenones, polyaromatic hydrocarbons, wine, cocoa butter) has been considered. It was found that the nebulizing efficiency of the LC-interfaces of the three detectors under consideration changes with the increasing liquid flow rate. For the MS, the increasing flow rate leads to a lower peak area whereas for the ELSD the peak area increases compared to the constant flow rate mode. The peak area obtained with a CAD is rather insensitive to the liquid flow rate. The reproducibility of the peak area remains similar in both modes, although variation in system permeability compromises the 'long-term' reproducibility. This problem can however be overcome by running a flow rate program with an optimized flow rate and composition profile obtained from the constant pressure mode. In this case, the quantification remains reproducibile, despite any occuring variations of the system permeability. Furthermore, the same fragmentation pattern (MS) has been found in the constant pressure mode compared to the customary constant flow rate mode.

  3. Intrinsic advantages of packed capillaries over narrow-bore columns in very high-pressure gradient liquid chromatography.

    Science.gov (United States)

    Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

    2016-06-17

    250μm×100mm fused silica glass capillaries were packed with 1.8μm high-strength silica (HSS) fully porous particles. They were prepared without bulky stainless steel endfittings and metal frits, which both generate significant sample dispersion. The isocratic efficiencies and gradient peak capacities of these prototype capillary columns were measured for small molecules (n-alkanophenones) using a home-made ultra-low dispersive micro-HPLC instrument. Their resolution power was compared to that of standard 2.1mm×100mm very high-pressure liquid chromatography (vHPLC) narrow-bore columns packed with the same particles. The results show that, for the same column efficiency (25000 plates) and gradient steepness (0.04min(-1)), the peak capacity of the 250μm i.d. capillary columns is systematically 15-20% higher than that of the 2.1mm i.d. narrow-bore columns. A validated model of gradient chromatography enabled one to predict accurately the observed peak capacities of the capillary columns for non-linear solvation strength retention behavior and under isothermal conditions. Thermodynamics applied to the eluent quantified the temperature difference for the thermal gradients in both capillary and narrow-bore columns. Experimental data revealed that the gradient peak capacity is more affected by viscous heating than the column efficiency. Unlike across 2.1mm i.d. columns, the changes in eluent composition across the 250μm i.d. columns during the gradient is rapidly relaxed by transverse dispersion. The combination of (1) the absence of viscous heating and (2) the high uniformity of the eluent composition across the diameter of capillary columns explains the intrinsic advantage of capillary over narrow-bore columns in gradient vHPLC.

  4. Quantification of clenbuterol at trace level in human urine by ultra-high pressure liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Nicoli, Raul; Petrou, Michael; Badoud, Flavia; Dvorak, Jiri; Saugy, Martial; Baume, Norbert

    2013-05-31

    Clenbuterol is a β2 agonist agent with anabolic properties given by the increase in the muscular mass in parallel to the decrease of the body fat. For this reason, the use of clenbuterol is forbidden by the World Anti-Doping Agency (WADA) in the practice of sport. This compound is of particular interest for anti-doping authorities and WADA-accredited laboratories due to the recent reporting of risk of unintentional doping following the eating of meat contaminated with traces of clenbuterol in some countries. In this work, the development and the validation of an ultra-high pressure liquid chromatography coupled to electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS) method for the quantification of clenbuterol in human urine is described. The analyte was extracted from urine samples by liquid-liquid extraction (LLE) in basic conditions using tert butyl-methyl ether (TBME) and analyzed by UHPLC-MS/MS with a linear gradient of acetonitrile in 9min only. The simple and rapid method presented here was validated in compliance with authority guidelines and showed a limit of quantification at 5pg/mL and a linearity range from 5pg/mL to 300pg/mL. Good trueness (85.8-105%), repeatability (5.7-10.6% RSD) and intermediate precision (5.9-14.9% RSD) results were obtained. The method was then applied to real samples from eighteen volunteers collecting urines after single oral doses administration (1, 5 and 10μg) of clenbuterol-enriched yogurts.

  5. Analysis of wax ester molecular species by high performance liquid chromatography/atmospheric pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Vrkoslav, Vladimír; Urbanová, Klára; Cvacka, Josef

    2010-06-18

    High chromatographic resolution of wax esters (WEs) was achieved by non-aqueous reversed-phase liquid chromatography on a Nova-Pak C18 column by optimising the acetonitrile/ethyl acetate mobile phase gradient. The retention behaviour of WEs was studied in this chromatographic system. The WEs eluted according to their equivalent carbon number (ECN) values; within the group of WEs with the identical ECN, the most unsaturated species tended to elute first. The isobaric WEs with different positions of the ester moiety were separated from each other whenever the lengths of the chains were sufficiently different. The methyl-branched esters eluted at shorter retention times than the straight-chained analogues, and the resolution among methyl-branched WEs depended on the position of the branching. The analytes were detected by atmospheric pressure chemical ionisation mass spectrometry (APCI-MS) using data-dependent scanning. WEs provided simple full-scan spectra with abundant protonated molecules and low-intensity fragments. Collision-induced dissociation (CID) promoted identification of the WE molecular species. The responses of WEs were found to be dependent on the number of double bonds and on the alkyl-chain length; the limits of the detection ranged from 20micromol/L to 200nmol/L. The HPLC/APCI-MS was applied for the analysis of the WEs isolated from honeycomb beeswax, jojoba oil and human hair. Good agreement between reported results and the literature data was achieved, with several novel polyunsaturated WEs also being found.

  6. Measurement of choline and choline metabolite concentrations using high-pressure liquid chromatography and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Pomfret, E A; daCosta, K A; Schurman, L L; Zeisel, S H

    1989-07-01

    We have developed a reproducible and sensitive procedure for the isolation and measurement of choline, phosphocholine, glycerophosphocholine, phosphatidylcholine, lysophosphatidylcholine and acetylcholine in a single 100-mg sample of biological tissue. Tissues were spiked with 14C-methyl- and 2H-methyl- or 15N-choline labeled internal standards for each compound. They were extracted with chloroform/methanol/water and the aqueous and organic phases were dried. The organic phase was resuspended in chloroform/methanol (1/1, v/v) and an aliquot was applied to a silica-gel thin-layer chromatography plate. The plate was developed in chloroform/methanol/water (65/30/4, v/v). Segments which cochromatographed with external standards of phosphatidylcholine and lysophosphatidylcholine were stained, scraped, and hydrolyzed in 6 M methanolic-HCl at 80 degrees C for 60 min, liberating free choline. The aqueous phase was resuspended in methanol/water and injected onto a silica HPLC column. Choline and its metabolites were eluted using a binary nonlinear gradient of acetonitrile/ethanol/acetic acid/1 M ammonium acetate/water/0.1 M sodium phosphate (800/68/2/3/127/10, v/v changing to 400/68/44/88/400/10, v/v). Peaks were detected with an on-line radiometric detector, collected, and dried under vacuum. Each choline ester was digested in 6 M HCl at 80 degrees C to form choline. Choline was then converted to the propionyl ester and demethylated with sodium benzenethiolate. This volatile derivative was then isolated using gas chromatography and measured with a mass selective detector. Deuterated internal standards were used to correct for variations in recovery. Choline, glycerophosphocholine, phosphocholine, phosphatidylcholine, lysophosphatidylcholine, and acetylcholine were measured in rat liver, heart, muscle, kidney, plasma, red blood cells, and brain and in human plasma.(ABSTRACT TRUNCATED AT 250 WORDS)

  7. Quasi-adiabatic vacuum-based column housing for very high-pressure liquid chromatography.

    Science.gov (United States)

    Gritti, Fabrice; Gilar, Martin; Jarrell, Joseph A

    2016-07-22

    A prototype vacuum-based (10(-6)Torr) column housing was built to thermally isolate the chromatographic column from the external air environment. The heat transfer mechanism is solely controlled by surface radiation, which was minimized by wrapping the column with low-emissivity aluminum tape. The adiabaticity of the column housing was quantitatively assessed from the measurement of the operational pressure and fluid temperature at the outlet of a 2.1mm×100mm column (sub-2 μm particles). The pressure drop along the column was raised up to 1kbar. The enthalpy balance of the eluent (water, acetonitrile, and one water/acetonitrile mixture, 70/30, v/v) showed that less than 1% of the viscous heat generated by friction of the fluid against the packed bed was lost to the external air environment. Such a vacuum-based column oven minimizes the amplitude of the radial temperature gradients across the column diameter and maximizes its resolving power.

  8. Determination of sedative hypnotics in sewage sludge by pressurized liquid extraction with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Arbeláez, Paula; Granados, Judith; Borrull, Francesc; Marcé, Rosa Maria; Pocurull, Eva

    2014-12-01

    This paper describes a method for the determination of eight sedative hypnotics (benzodiazepines and barbiturates) in sewage sludge using pressurized liquid extraction and liquid chromatography with tandem mass spectrometry. Pressurized liquid extraction operating conditions were optimized and maximum recoveries were reached using methanol under the following operational conditions: 100ºC, 1500 psi, extraction time of 5 min, one extraction cycle, flush volume of 60% and purge time of 120 s. Pressurized liquid extraction recoveries were higher than 88% for all the compounds except for carbamazepine (55%). The repeatability and reproducibility between days, expressed as relative standard deviation (n = 5), were lower than 6 and 10%, respectively. The detection limits for all compounds were lower than 12.5 μg/kg of dry weight. The method was applied to determine benzodiazepines and barbiturates in sewage sludge from urban sewage treatment plants, and carbamazepine showed the highest concentration (7.9-18.9 μg/kg dry weight).

  9. Determination of potato glycoalkaloids using high-pressure liquid chromatography-electrospray ionisation/mass spectrometry.

    Science.gov (United States)

    Matsuda, Fumio; Morino, Keiko; Miyazawa, Haruna; Miyashita, Masahiro; Miyagawa, Hisashi

    2004-01-01

    A method for quantifying two toxic glycoalkaloids, alpha-solanine and alpha-chaconine, in potato (Solanum tuberosum) tuber tissue was developed using HPLC-electrospray ionisation (ESI)/MS. Potato samples were extracted with 5% aqueous acetic acid, and the extracts were subjected directly to HPLC-ESI/MS after filtration. By determining the intensities of the protonated molecules of alpha-solanine (m/z 868) and alpha-chaconine (m/z 852) using selected ion monitoring (positive ion mode), a sensitive assay was attained with detection limits of 38 and 14 ppb for the two glycoalkaloids, respectively. The high sensitivity and selectivity of MS detection effectively reduced the time of analysis thus enabling a high throughput assay of glycoalkaloids in potato tubers.

  10. High-performance liquid chromatography of biopolymers

    Energy Technology Data Exchange (ETDEWEB)

    Regnier, F.E.

    1983-10-21

    The ability to separate biological macromolecules with good resolution on liquid chromatographic columns has depended on the development of suitable packing materials. In size exclusion chromatography, molecules are separated by size on the basis of differential permeation of the packing. Ion exchange, hydrophobic interaction (or reversed-phase), and affinity chromatography are all surface-mediated separation methods, although they depend on different retention mechanisms. High-performance liquid chromatographic columns designed for biopolymers offer major advantages over conventional columns in both speed and resolving power. The exponential growth of literature on the high-performance separation of peptides and proteins in particular indicates that the techniques will become the dominant form of column liquid chromatography. 92 refs., 4 figs.

  11. Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with pressurized liquid extraction for simultaneous quantification and confirmation of cyromazine, melamine and its metabolites in foods of animal origin

    Energy Technology Data Exchange (ETDEWEB)

    Yu Huan; Tao Yanfei; Chen Dongmei; Wang Yulian; Liu Zhaoying; Pan Yuanhu; Huang Lingli; Peng Dapeng; Dai Menghong; Liu Zhenli [MOA Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei 430070 (China); Yuan Zonghui, E-mail: yuan5802@mail.hzau.edu.cn [MOA Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei 430070 (China)

    2010-12-03

    Simple and sensitive methods have been developed for simultaneous detection of cyromazine, melamine and their metabolites (ammeline, ammelide and cyanuric acid) in samples of animal origins. These include a high performance liquid chromatography (HPLC) method and a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method and are useful in regular monitoring and in toxicity studies of these molecules. Representative samples used in this study include muscles and livers of swine, bovine, sheep and chicken, kidneys of swine, bovine and sheep, and milk powder. A new sample preparation procedure with pressurized liquid extraction (PLE) at 1400 psi and 70 deg. C was investigated. Quantification of these five compounds by HPLC was achieved using an APS-2 column with UV detection at 230 nm. Limit of detection (LOD) was at 10 {mu}g kg{sup -1}, and limit of quantification (LOQ) was at 40 {mu}g kg{sup -1}. Recoveries of the five analytes in spiked samples ranged from 72.2% to 115.4% with RSD less than 12%. Confirmatory analysis of the analytes was performed using LC-MS/MS in selected reaction monitoring (SRM) mode. The LOD and LOQ were 5 {mu}g kg{sup -1} and 15 {mu}g kg{sup -1}, respectively. This is the first simultaneous analysis of cyromazine, melamine, ammeline, ammelide and cyanuric acid residues in complex tissue samples using PLE and HPLC. It is expected that these methods will find many practical applications in evaluating the safety of cyromazine, melamine and their metabolites.

  12. High Performance Liquid Chromatography/Video Fluorometry. Part I. Instrumentation.

    Science.gov (United States)

    1981-09-30

    High Performance Liquid Chromatography /Video...PERIOD COVERED High Performance Liquid Chromatography /Video .. / Fluorometry. Part I. Instrumentation. . Interim/ echnicaliepart,. 6. PERFORMING ORG...34Entered SECURITY CLASSIFICATION OF THIS OlAGE (When Data Entered) II1| III I I I I E I II ... .. High Performance Liquid Chromatography

  13. Basic prinicipal of high performance liquid chromatography

    OpenAIRE

    Ivanova, Violeta

    2016-01-01

    High-performance liquid chromatography (HPLC) is an analytical technique based on the separation of molecules due to differences in their structure and/or composition. Separation is performed between two phases, mobile and stationary. The molecules in the sample have different affinities and interactions with the stationary support, leading to separation of molecules. Compounds which are longer retained at the stationary phase will elute later, compared to those which are distributed into the...

  14. Fast analysis of 29 polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs with ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry

    OpenAIRE

    Shih-Chun Candice Lung; Chun-Hu Liu

    2015-01-01

    Polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs are ubiquitous in the environment. Some of them are probable carcinogens and some are source markers. This work presents an ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry (UHPLC-APPI-MS/MS) method for simultaneous analysis of 20 PAHs and nine nitro-PAHs. These compounds are separated in 15 minutes in the positive mode and 11 minutes in the negative mode, one half of GC/MS analysi...

  15. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection in the analysis of agrochemical residues and mycotoxins in food - challenges and applications.

    Science.gov (United States)

    O'Mahony, John; Clarke, Lesa; Whelan, Michelle; O'Kennedy, Richard; Lehotay, Steven J; Danaher, Martin

    2013-05-31

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence of UHPLC through technological advances. The implications of this new chromatographic technology for MS detection are discussed, as well as some of the remaining challenges in exploiting it for chemical residue applications. Finally, a comprehensive overview of published applications of UHPLC-MS in food contaminant analysis is presented, with a particular focus on veterinary drug residues.

  16. Determination of Essential Fatty Acid Composition among Mutant Lines of Canola (Brassica napus), through High Pressure Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    Ghulam Raza; Aquil Siddique; Imtiaz Ahmad Khan; Muhammed Yasin Ashraf; Abdullah Khatri

    2009-01-01

    The present study aimed to quantify the methyl esters of lenoleic acid (LA), γ-lenolenic acid (LNA) and oleic acid (OL) in the oil of Brassica napus mutants. Five stable mutants (ROO-75/1, ROO-100/6, ROO-125/12, ROO-125/14, and ROO-125/17)of B. napus cv. 'Rainbow' (P) and three mutants (W97-95116, W97-0.75/11 and W97-.075/13) of B. napus cv. 'Westar' (P) at M6 stage, exhibiting better yield and yield components, were analyzed for essential fatty acids. The highest seed yield was observed in the mutant (ROO-100/6) followed by ROO-125/14 of Rainbow, that is, 34% and 32% higher than their parent plants, respectively. Westar mutant W97-75/11 also showed 30% higher seed yield than its parent plant. High performance liquid chromatography analysis of the composition of fatty acids indicated that OL was the most dominant fatty acid, ranging from 39.1 to 66.3%; LA was second (15.3-41.6%) and LNA was third (18.1-28.9%). Mutant ROO-125/14 showed higher OL contents than parent (Rainbow). These results are expected to support the approval of ROO-125/14 in the National Uniform Varietal Yield Trials (NUVYT) as a new variety based on high oil quality.

  17. Multicomponent mixed dopant optimization for rapid screening of polycyclic aromatic hydrocarbons using ultra high performance liquid chromatography coupled to atmospheric pressure photoionization high-resolution mass spectrometry

    KAUST Repository

    Sioud, Salim

    2012-05-04

    RATIONALE To enhance the ionization efficiencies in atmospheric pressure photoionization mass spectrometry a dopant with favorable ionization energy such as chlorobenzene is typically used. These dopants are typically toxic and difficult to mix with water-soluble organic solvents. In order to achieve a more efficient and less toxic dopant, a multicomponent mixed dopant was explored. METHODS A multicomponent mixed dopant for non-targeted rapid screening of polycyclic aromatic hydrocarbons (PAHs) was developed and optimized using ultra high performance liquid chromatography (UPLC) coupled to atmospheric pressure photoionization high-resolution mass spectrometry. Various single and multicomponent mixed dopants consisting of ethanol, chlorobenzene, bromobenzene, anisole and toluene were evaluated. RESULTS Fourteen out of eighteen PAHs were successfully separated and detected at low pg/μL levels within 5 min with high mass accuracy ≤4 ppm. The optimal mixed multicomponent dopant consisted of ethanol/chlorobenzene/bromobenzene/anisole (98.975:0.1:0.9:0.025, v/v %) and it improved the limit of detection (LOD) by 2- to 10-fold for the tested PAHs compared to those obtained with pure chlorobenzene. CONCLUSIONS A novel multicomponent dopant that contains 99% ethanol and 1% mixture of chlorobenzene, bromobenzene and anisole was found to be an effective dopant mixture to ionize PAHs. The developed UPLC multicomponent dopant assisted atmospheric pressure photoionization high-resolution mass spectrometry offered a rapid non targeted screening method for detecting the PAHs at low pg/;μL levels within a 5 min run time with high mass accuracy a;circ4 ppm. Copyright © 2012 John Wiley & Sons, Ltd.

  18. A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Russo, Mariateresa; Valdés, Alberto; Ibáñez, Clara; Rastrelli, Luca

    2015-04-01

    According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30%) at 110 °C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103%) and repeatability (RSD < 8, n = 3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling high-throughput analysis and highly accurate and precise results.

  19. A highly specific and sensitive quantification analysis of the sterols in silkworm larvae by high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.

    Science.gov (United States)

    Igarashi, Fumihiko; Hikiba, Juri; Ogihara, Mari H; Nakaoka, Takayoshi; Suzuki, Minoru; Kataoka, Hiroshi

    2011-12-15

    The biochemical quantification of sterols in insects has been difficult because only small amounts of tissues can be obtained from insect bodies and because sterol metabolites are structurally related. We have developed a highly specific and sensitive quantitative method for determining of the concentrations of seven sterols-7-dehydrocholesterol, desmosterol, cholesterol, ergosterol, campesterol, stigmasterol, and β-sitosterol-using a high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (HPLC/APCI-MS/MS). The sterols were extracted from silkworm larval tissues using the Bligh and Dyer method and were analyzed using HPLC/APCI-MS/MS with selected reaction monitoring, using cholesterol-3,4-(13)C(2) as an internal standard. The detection limits of the method were between 12.1 and 259 fmol. The major sterol in most silkworm larval tissues was cholesterol, whereas only small quantities of the dietary sterols were detected. Thus, a simple, sensitive, and specific method was successfully developed for the quantification of the sterol concentrations in each tissue of an individual silkworm larva. This method will be a useful tool for investigating to molecular basis of sterol physiology in insects, facilitating the quantification of femtomole quantities of sterols in biological samples.

  20. Determination of Selected Colored Smokes on Glass Fiber Discs by High Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    1991-05-01

    High Performance Liquid Chromatography (HPLC) 12. PERSONAL AUTHOR(S) F F_ n.ipl’prifl. Alan R...GROUP SUB-GROUP High Performance Liquid Chromatography (HPLC), Analytical IMethod, 1,4-diamino-2,3-dihydroanthraquinone, 2-(2 - _ quinolinyl)-1,3...weights, low vapor pressures and low thermal stability. High performance liquid chromatography (HPLC) appears to be the analytical method of choice

  1. High Performance Liquid Chromatography/Video Fluorometry. Part II. Applications.

    Science.gov (United States)

    1981-09-30

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY /VIDEO FLUOROMETRY. PART...REP«T_N&:-ŗ/ High Performance Liquid Chromatography /Video Fluorometry» Part II. Applications« by | Dennis C./Shelly* Michael P./Vogarty and...Data EnlirtdJ REPORT DOCUMENTATION PAGE t. REPORT NUMBER 2 GOVT ACCESSION NO 4. T1TI.F (and Submit) lP-^fffsyva High Performance Liquid Chromatography

  2. Analysis of oxysterols and vitamin D metabolites in mouse brain and cell line samples by ultra-high-performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry.

    Science.gov (United States)

    Ahonen, Linda; Maire, Florian B R; Savolainen, Mari; Kopra, Jaakko; Vreeken, Rob J; Hankemeier, Thomas; Myöhänen, Timo; Kylli, Petri; Kostiainen, Risto

    2014-10-17

    We have developed an ultra-high-performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometric (UHPLC-APPI-MS/MS) method for the simultaneous quantitative analyses of several oxysterols and vitamin D metabolites in mouse brain and cell line samples. An UHPLC-APPI-high resolution mass spectrometric (UHPLC-APPI-HRMS) method that uses a quadrupole-time of flight mass spectrometer was also developed for confirmatory analysis and for the identification of non-targeted oxysterols. Both methods showed good quantitative performance. Furthermore, APPI provides high ionization efficiency for determining oxysterols and vitamin D related compounds without the time consuming derivatization step needed in the conventionally used electrospray ionization method to achieve acceptable sensitivity. Several oxysterols were quantified in mouse brain and cell line samples. Additionally, 25-hydroxyvitamin D3 was detected in mouse brain samples for the first time.

  3. Comparison of different calibration approaches for chloramphenicol quantification in chicken muscle by ultra-high pressure liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Pan, Xiao-Dong; Jiang, Wei; Wu, Ping-Gu

    2015-01-07

    Matrix-dependent signal suppression often occurs in quantitative analysis by ultra-high pressure liquid chromatography tandem mass spectrometry (UPLC-MS/MS). In this study, we investigated three calibration methods for compensation of signal suppression on chloramphenicol (CAP) quantification in chicken muscle. The data showed that the spiking recoveries by solvent standard calibration with a stable isotope labelled internal standard (SIL-IS) and matrix-matched standard calibration with a SIL-IS were significantly higher than by external matrix-matched standard calibration (P 0.05). The limit of detection (LOD) for external matrix matched standard calibration was 0.1 μg kg(-1), and that for SIL-IS calibration (including matrix matched and solvent dissolved standard) was 0.03 μg kg(-1).

  4. Thermal expansion pump for capillary high-performance liquid chromatography.

    Science.gov (United States)

    Tao, Qian; Wu, Qian; Zhang, Xiangmin

    2010-02-01

    A thermal expansion pump (TEP) based on a principle of liquid thermal expansion for capillary high-performance liquid chromatography has been developed. The novel pump is capable of generating a continuous flow at high pressure for constant and stable delivery of binary solvents from nanoliters to microliters per minute without splitting. Theoretical equations for controlling fluidic output of this pump have been established and validated by a series of experiments. Factors affecting flow rate, such as density discrepancy, liquid compressibility, and mass loss in output, were taken into account. An assembly of the pump system employing two groups of thermal expansion pumps (TEPs) working in turns were fabricated, and a controlling strategy for the pump system to maintain a continuous delivery without pressure fluctuation even at switching points was also developed. Both isocratic and gradients of binary solvent delivery by the TEPs were performed. Reproducibility and standard deviation at different flow rates were determined. A capillary high-performance liquid chromatography (micro-HPLC) system consisting of the TEPs, an injection valve, a homemade packed capillary column (20 cm x 100 microm i.d. with 5 microm C18), and a laser-induced fluorescence detector was set up, and sample separations were carried out. Results of RSD = 4% for flow and RSD = 2% for retention times at 500 nL/min were achieved. Such a pump system has almost no moving parts except for the solvent switches. Its overall costs of manufacture and running are very low. It is proven that the TEPs system has great potential and competitive capabilities in capillary liquid chromatography.

  5. High-Performance Liquid Chromatography: An Overview

    OpenAIRE

    Tandia N; Singh SK1; Kumar N; Singh S

    2013-01-01

    Chromatography is considered extremely powerful separation technique for variety of samples. Thecommon feature of all these techniques is that the different components in a sample mixture aredistributed between two phases, one of which remains stationary while the other the mobile phase, runsthrough the interstices or over the surface of the fixed phase. The movement of the mobile phase resultsin differential migration of the sample components. High performance thin layer chromatography is an...

  6. Simultaneous pressurized enzymatic hydrolysis extraction and clean up for arsenic speciation in seafood samples before high performance liquid chromatography-inductively coupled plasma-mass spectrometry determination.

    Science.gov (United States)

    Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; Moreda-Piñeiro, Antonio; Moscoso-Pérez, Carmen; Muniategui-Lorenzo, Soledad; López-Mahía, Purificación; Prada-Rodríguez, Darío; Bermejo-Barrera, Pilar

    2010-10-29

    The feasibility of pressurized conditions to assist enzymatic hydrolysis of seafood tissues for arsenic speciation was novelty studied. A simultaneous in situ (in cell) clean-up procedure was also optimized, which speeds up the whole sample treatment. Arsenic species (As(III), MMA, DMA, As(V), AsB and AsC) were released from dried seafood tissues using pepsin as a protease, and the arsenic species were separated/quantified by anion exchange high performance liquid chromatography (HPLC) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). Variables inherent to the enzymatic activity (pH, temperature and ionic strength), the amount of enzyme (pepsin), and factors affecting pressurization (pressure, static time, number of cycles and amount of dispersing agent, C-18) were fully evaluated. Pressurized assisted enzymatic hydrolysis (PAEH) with pepsin can be finished after few minutes (two cycles of 2 min each one plus 3 min to reach the hydrolysis temperature of 50 °C). A total sample solubilisation is not achieved after the procedure, however it is efficient enough for breaking down certain bonds of bio-molecules and for releasing arsenic species. The developed method has been found to be precise (RSDs lower than 6% for As(III), DMA and As(V); and 3% for AsB) and sensitive (LOQs of 18.1, 36.2, 35.7, 28.6, 20.6 and 22.5 ng/g for As(III), MMA, DMA, As(V), AsB and AsC, respectively). The optimized methodology was successfully applied to different certified reference materials (DORM-2 and BCR 627) which offer certified AsB and DMA contents, and also to different seafood products (mollusks, white fishes and cold water fishes).

  7. Trends in High Performance Liquid Chromatography for Cultural Heritage.

    Science.gov (United States)

    Degano, Ilaria; La Nasa, Jacopo

    2016-04-01

    The separation, detection and quantitation of specific species contained in a sample in the field of Cultural Heritage requires selective, sensitive and reliable methods. Procedures based on liquid chromatography fulfil these requirements and offer a wide range of applicability in terms of analyte types and concentration range. The main applications of High Performance Liquid Chromatography in this field are related to the separation and detection of dyestuffs in archaeological materials and paint samples by reversed-phase liquid chromatography with suitable detectors. The relevant literature will be revised, with particular attention to sample treatment strategies and future developments. Reversed phase chromatography has also recently gained increasing importance in the analysis of lipid binders and lipid materials in archaeological residues: the main advantages and disadvantages of the new approaches will be discussed. Finally, the main applications of ion chromatography and size exclusion chromatography in the field of Cultural Heritage will be revised in this chapter.

  8. Fast analysis of 29 polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs with ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry

    Science.gov (United States)

    Lung, Shih-Chun Candice; Liu, Chun-Hu

    2015-08-01

    Polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs are ubiquitous in the environment. Some of them are probable carcinogens and some are source markers. This work presents an ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry (UHPLC-APPI-MS/MS) method for simultaneous analysis of 20 PAHs and nine nitro-PAHs. These compounds are separated in 15 minutes in the positive mode and 11 minutes in the negative mode, one half of GC/MS analysis time. Two pairs of precursor/product ions are offered, which is essential for confirmation. This method separates and quantifies benzo[a]pyrene (the most toxic PAHs) and non-priority benzo[e]pyrene (isomers, little toxicity) to avoid overestimation of toxin levels, demonstrating its importance for health-related researches. With 0.5% 2,4-difluoroanisole in chlorobenzene as the dopant, limits of detection of PAHs except acenaphthylene and those of nitro-PAHs except 2-nitrofluoranthene are below 10 pg and 3 pg, respectively, mostly lower than or comparable to those reported using LC-related systems. The responses were linear over two orders of magnitude with fairly good accuracy and precision. Certified reference materials and real aerosol samples were analyzed to demonstrate its applicability. This fast, sensitive, and reliable method is the first UHPLC-APPI-MS/MS method capable of simultaneously analyzing 29 environmentally and toxicologically important PAHs and nitro-PAHs.

  9. Reaction profiling by ultra high-pressure liquid chromatography/time-of-flight mass spectrometry in support of the synthesis of DNA-encoded libraries.

    Science.gov (United States)

    Hargiss, Leonard O; Zipp, G Greg; Jessop, Theodore C; Sun, Xuejun; Keyes, Philip; Rawlins, David B; Liang, Zhi; Park, Kum Joo; Gu, Huizhong

    2014-11-15

    An ultra high-pressure liquid chromatography/mass spectrometry (UHPLC/MS) separation and analysis method has been devised for open access analysis of synthetic reactions used in the production of DNA-encoded chemical libraries. The aqueous mobile phase is 100mM hexafluoroisopropanol and 8.6mM triethylamine; the organic mobile phase is methanol. The UHPLC separation uses a C18 OST column (50mm×2.1mm×1.7μm) at 60°C, with a flow rate of 0.6mL/min. Gradient concentration is from 10 to 40% B in 1.0min, increasing to 95% B at 1.2min. Cycle time was about 5min. This method provides a detection limit of a 20-mer oligonucleotide by mass spectrometry of better than 1pmol on-column. Linear UV response for 20-mer extends from 2 to 200pmol/μL in concentration, same-day relative average deviations are less than 5% and bias (observed minus expected) is less than 10%. Deconvoluted mass spectra are generated for components in the predicted mass range using a maximum entropy algorithm. Mass accuracy of deconvoluted spectra is typically 20ppm or better for isotopomers of oligonucleotides up to 7000Da.

  10. In vivo biosynthesis of L-(/sup 35/S)Cys-arginine vasopressin, -oxytocin, and -somatostatin: rapid estimation using reversed phase high pressure liquid chromatography. [Rats

    Energy Technology Data Exchange (ETDEWEB)

    Franco-Bourland, R.E.; Fernstrom, J.D.

    1981-01-01

    L(/sup 35/S)Cys-arginine vasopressin, -oxytocin, and -somatostatin were purified from hypothalami and neurohypophyses 4 h after rats received L(/sup 35/S)Cys via the third ventricle. After acetic acid extraction, Sephadex G-25 filtration, and chemoadsorption to C18-silica (Sep-Pak cartridges), the labeled peptides were rapidly separated by gradient elution, reversed phase, high pressure liquid chromatography (HPLC). The identity and isotopic purity of the labeled peptides were determined by several reversed phase HPLC procedures in conjunction with chemical modification. The labeled peptide fractions were at least 50% radiochemically pure. Using this HPLC isolation procedure, incorporation of L-(/sup 35/S)Cys into each peptide was determined in hydrated and dehydrated rats. Label incorporation into arginine vasopressin and oxytocin in the hypothalamus and the neurohypophysis of dehydrated rats was 2-3 times greater than that in hydrated rats. Incorporation of label into hypothalamic and neurohypophyseal somatostatin was unaffected by the hydration state of the animal. This procedure thus provides a very rapid, but sensitive, set of techniques for studying the control of small peptide biosynthesis in the brain.

  11. Energy metabolism during microsurgical transfer of human skeletal muscle assessed by high-pressure liquid chromatography and by 31P-nuclear magnetic resonance.

    Science.gov (United States)

    Lundberg, Jonas; Elander, Anna; Rakotonirainy, Olivier; Zetterlund, Therese; Fogdestam, Ingemar; Soussi, Bassam

    2002-01-01

    The effect of ischaemia and reperfusion on human skeletal muscle was studied during free vascularised muscle transfer. Muscle biopsy specimens were taken from patients having microsurgical muscle transfer, 18 cases (17 patients; 12 men, 5 women). The biopsies were taken three times: before transfer of the muscle (control), at maximum ischaemic time, and one hour after revascularisation. The biopsy specimens were analysed for purine nucleotides, by high-pressure liquid chromatography (HPLC), and by nuclear magnetic resonance (NMR) at 500 MHz. Phosphocreatine (PCr) recovered only partially (79%) and adenosine triphosphate (ATP) did not differ significantly from normal control after revascularisation and a mean ischaemic time of 114 minutes. NMR measurements showed an accumulation of glucose-6-phosphate (G-6-P) during the ischaemic period, indicating anaerobic metabolism. After three hours of ischaemia and one hour of reperfusion the PCr recovery was less than 60% (r = 0.7). The results confirm those of previous animal studies, which set three hours normothermic ischaemia as a safe limit for tissue preservation when transferring skeletal muscle. Longer ischaemic times may cause serious postoperative healing problems and reduced muscle function.

  12. Fast analysis of 29 polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs with ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry.

    Science.gov (United States)

    Lung, Shih-Chun Candice; Liu, Chun-Hu

    2015-08-12

    Polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs are ubiquitous in the environment. Some of them are probable carcinogens and some are source markers. This work presents an ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry (UHPLC-APPI-MS/MS) method for simultaneous analysis of 20 PAHs and nine nitro-PAHs. These compounds are separated in 15 minutes in the positive mode and 11 minutes in the negative mode, one half of GC/MS analysis time. Two pairs of precursor/product ions are offered, which is essential for confirmation. This method separates and quantifies benzo[a]pyrene (the most toxic PAHs) and non-priority benzo[e]pyrene (isomers, little toxicity) to avoid overestimation of toxin levels, demonstrating its importance for health-related researches. With 0.5% 2,4-difluoroanisole in chlorobenzene as the dopant, limits of detection of PAHs except acenaphthylene and those of nitro-PAHs except 2-nitrofluoranthene are below 10 pg and 3 pg, respectively, mostly lower than or comparable to those reported using LC-related systems. The responses were linear over two orders of magnitude with fairly good accuracy and precision. Certified reference materials and real aerosol samples were analyzed to demonstrate its applicability. This fast, sensitive, and reliable method is the first UHPLC-APPI-MS/MS method capable of simultaneously analyzing 29 environmentally and toxicologically important PAHs and nitro-PAHs.

  13. Physicochemical and thermodynamic characterization of the encapsulation of methyl jasmonate by natural and modified cyclodextrins using reversed-phase high-pressure liquid chromatography.

    Science.gov (United States)

    López-Nicolás, José Manuel; Escorial Camps, Marta; Pérez-Sánchez, Horacio; García-Carmona, Francisco

    2013-11-27

    Although the combinations of methyl jasmonate (MeJA) and cyclodextrins (CDs) have been used by different authors to stimulate the production of several metabolites, no study has been published about the possible formation of MeJA-CD complexes when these two molecules are added together to the reaction medium as elicitors. For this reason and because knowledge of the possible complexation process of MeJA with CD under different physicochemical conditions is essential if these two molecules are to be used in cell cultures, this paper looks at the complexation of MeJA with natural and modified CDs using a reversed-phase high-pressure liquid chromatography (RP-HPLC) system. The interaction of MeJA with β-CD was more efficient than with α- and γ-CDs. However, a modified CD, HP-β-CD, was the most effective of all of the CDs tested. Moreover, MeJA formed complexes with CD with a 1:1 stoichiometry, and the formation constants of these complexes were strongly dependent upon the temperature of the mobile phase used but not the pH. To obtain information about the mechanism of the affinity of MeJA for CD, the thermodynamic parameters ΔG°, ΔH°, and ΔS° were calculated. Finally, molecular modeling studies were carried out to propose which molecular interactions are established in the complexation process.

  14. Exploring in vitro neurobiological effects and high-pressure liquid chromatography-assisted quantitation of chlorogenic acid in 18 Turkish coffee brands

    Directory of Open Access Journals (Sweden)

    Sinem Aslan Erdem

    2016-01-01

    Full Text Available The hydroalcoholic extracts of the Turkish traditional coffee samples from 18 commercial brands were tested for their neurobiological effects through enzyme inhibition based on enzyme-linked immunosorbance microtiter assays against acetylcholinesterase, butyrylcholinesterase, and tyrosinase, linked to Alzheimer's and Parkinson's diseases. The extracts were also subjected to several antioxidant test systems to define their antiradical, metal-chelation capacity, and reducing power. Total phenol and flavonoid contents in the extracts were delineated by spectrophotometric methods, while chlorogenic acid in the coffee samples was quantified by high-pressure liquid chromatography. The extracts displayed low to moderate inhibition (from 2.13 ± 0.01% to 36.12 ± 1.07% at 200 μg/mL against the tested enzymes, whereas they had notable 2,2′-diphenyl-1-picrylhydrazyl radical scavenging activity up to 56.15 ± 2.03% at 200 μg/mL. The extracts exerted a remarkable ferric-reducing antioxidant power values, while chlorogenic acid was found to range between 0.288 ± 0.005% and 2.335 ± 0.010%.

  15. Simultaneous determination of some phthalate metabolites, parabens and benzophenone-3 in urine by ultra high pressure liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Dewalque, Lucas; Pirard, Catherine; Dubois, Nathalie; Charlier, Corinne

    2014-02-15

    Phthalates, parabens and 2-hydroxy-4-methoxybenzophenone or benzophone-3 are thought to act as endocrine disrupting chemicals, being able to disrupt the endocrine balance and therefore able to lead to some hormonal diseases. Numerous large-scale biomonitoring studies have detected the biomarkers of these compounds in more than 75% of the general population. To assess the exposure to these chemicals, we developed an analytical method based on a Solid Phase Extraction (SPE) prior to ultra high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous measurement of seven phthalate metabolites (monobenzyl phthalate, mono-n-butyl phthalate, mono-iso-butyl phthalate, mono-2-ethylhexyl phthalate, mono-2-ethyl-5-hydroxyhexyl phthalate, mono-2-ethyl-5-oxohexyl phthalate, monoethyl phthalate), four parabens (methyl paraben, ethyl paraben, n-propyl paraben, n-butyl parabens) and benzophenone-3 in human urine. The distinction between unconjugated, glucuro- and sulfoconjugated forms was achieved using different enzymatic hydrolyses. The whole procedure was validated according to the total error approach, and was demonstrated to be linear (regression coefficient ranging from 0.987 to 0.998) and accurate (inter and intra assay precision parabens and benzophenone-3 were positively detected in almost all urine samples, with detection rates ranging from 40 to 100%. Levels measured ranged from parabens and benzophenone-3 were detected as glucuro- and sulfoconjugated species in variable proportions according to the target compound.

  16. An ultra-high pressure liquid chromatography-tandem mass spectrometry method for the quantification of teicoplanin in plasma of neonates.

    Science.gov (United States)

    Begou, O; Kontou, A; Raikos, N; Sarafidis, K; Roilides, E; Papadoyannis, I N; Gika, H G

    2016-02-04

    The development and validation of an ultra-high pressure liquid chromatography (UHPLC) tandem mass spectrometry (MS/MS) method was performed with the aim to be applied for the quantification of plasma teicoplanin concentrations in neonates. Pharmacokinetic data of teicoplanin in the neonatal population is very limited, therefore, a sensitive and reliable method for the determination of all isoforms of teicoplanin applied in a low volume of sample is of real importance. Teicoplanin main components were extracted by a simple acetonitrile precipitation step and analysed on a C18 chromatographic column by a triple quadrupole MS with electrospray ionization. The method provides quantitative data over a linear range of 25-6400ng/mL with LOD 8.5ng/mL and LOQ 25ng/mL for total teicoplanin. The method was applied in plasma samples from neonates to support pharmacokinetic data and proved to be a reliable and fast method for the quantification of teicoplanin concentration levels in plasma of infants during therapy in Intensive Care Unit.

  17. Analysis of Tocopherols by High Performance Liquid Chromatography

    OpenAIRE

    Edison, B.

    2009-01-01

    : Gas chromatography is the key technique for organic components and also for tocopherols analysis. High performance liquid chromatography has an important role to take part in applications such as the handling of less usual samples, prevention of degradation of heat sensitive functional groups and for micro preparative purposes. Many approaches for development of improved methods are suggested, especially for reversed phase applications.

  18. Pressurized liquid extraction followed by liquid chromatography with tandem mass spectrometry to determine pharmaceuticals in mussels.

    Science.gov (United States)

    Núñez, Mireia; Borrull, Francesc; Pocurull, Eva; Fontanals, Núria

    2016-02-01

    An analytical method based on pressurized liquid extraction and solid-phase extraction with a mixed-mode Oasis(®) MAX sorbent as cleanup, followed by liquid chromatography with electrospray ionization and tandem mass spectrometry was developed and validated for the determination of seven widely used pharmaceuticals in mussel species. The optimization of the pressurized liquid extraction and the solid-phase extraction parameters is described. The method provided extraction recoveries ranging from 61 to 90%, and limits of detection ranging from 2 to 50 ng/g (dry weight). The repeatability and reproducibility of the method, expressed as relative standard deviation, were lower than 15 and 19%, respectively. The method was successfully applied to the analysis of mussel samples from different locations. The analyses showed that salicylic acid was present in mussels at concentrations up to 177 ng/g (dry weight).

  19. Profiling of triacylglycerols in plant oils by high-performance liquid chromatography-atmosphere pressure chemical ionization mass spectrometry using a novel mixed-mode column.

    Science.gov (United States)

    Hu, Na; Wei, Fang; Lv, Xin; Wu, Lin; Dong, Xu-Yan; Chen, Hong

    2014-12-01

    In this investigation, a rapid and high-throughput method for profiling of TAGs in plant oils by liquid chromatography using a single column coupled with atmospheric pressure chemical ionization (APCI) mass spectrometry was reported. A novel mixed-mode phenyl-hexyl chromatographic column was employed in this separation system. The phenyl-hexyl column could provide hydrophobic interactions as well as π-π interactions. Compared with two traditionally columns used in TAG separation - the C18 column and silver-ion column, this column exhibited much higher selectivity for the separation of TAGs with great efficiency and rapid speed. By comparison with a novel mix-mode column (Ag-HiSep OTS column), which can also provide both hydrophobic interactions as well as π-π interactions for the separation of TAGs, phenyl-hexyl column exhibited excellent stability. LC method using phenyl-hexyl column coupled with APCI-MS was successfully applied for the profiling of TAGs in soybean oils, peanut oils, corn oils, and sesame oils. 29 TAGs in peanut oils, 22 TAGs in soybean oils, 19 TAGs in corn oils, and 19 TAGs in sesame oils were determined and quantified. The LC-MS data was analyzed by barcodes and principal component analysis (PCA). The resulting barcodes constitute a simple tool to display differences between different plant oils. Results of PCA also enabled a clear identification of different plant oils. This method provided an efficient and convenient chromatographic technology for the fast characterization and quantification of complex TAGs in plant oils at high selectivity. It has great potential as a routine analytical method for analysis of edible oil quality and authenticity control.

  20. Structures of Liquid Aluminium under High Pressure

    Institute of Scientific and Technical Information of China (English)

    LI Hui; WANG Guang-Hou; BIAN Xiu-Fang; ZHANG Lin

    2001-01-01

    Molecular dynamics simulation has been carried out for melt A1 under constant temperature and constant pressure. The interaction between atoms is described by tight-binding many-body potentials based on the second moment approximation to the electronic density of states. The pair correlation function and the pair analysis technique are used to reveal the structural features of liquid Al under normal and high pressure. High pressure is favourable to the existence of bcc clusters 1661 and 1441, but has no effect on the fcc cluster 1421. The bond pair 1551 and 1541 with fivefold symmetry exists at high pressure. The microstructure of liquid is more similar to the non-crystalline structure than to the crystalline structure. The simulation results are supported by thex-ray experimental results.

  1. Determination of Glucosamine in Human Plasma by High-Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization Source-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xingchen Zhou

    2011-01-01

    Full Text Available A sensitive, specific, and rapid high-performance liquid chromatography-atmospheric pressure chemical ionization source-tandem mass spectrometry (HPLC-APCI-MS/MS method for the determination of glucosamine in human plasma was developed and validated. Plasma samples were processed by protein precipitation with dehydrated ethanol, and the chromatographic separation was performed on an Agilent XDB-C18 column with a mobile phase of methanol—0.2% formic acid solution (70 : 30, v/v. Mass spectrometric quantification was carried out in the multiple reaction monitoring (MRM mode, monitoring ion transitions of m/z 180.1 to m/z 162.1 with collision energy (CE of 2 eV for glucosamine and m/z 181.1 to m/z 163.1 with CE of 2 eV for the internal standard (IS in positive ion mode. The linear calibration curves covered a concentration range of 53.27–3409 ng/mL with a lower limit of quantification (LLOQ of 53.27 ng/mL. The extraction recovery of glucosamine was greater than 101.7%. The intra- and interday precisions for glucosamine were less than 10%, and the accuracies were between 93.7% and 102.6%, determined from quality control (QC samples of three representative concentrations. The method has been successfully applied to determining the plasma concentration of glucosamine in a clinical pharmacokinetic study involving 20 healthy Chinese male volunteers.

  2. Radiocarbon Analysis of Individual Amino Acids: Carbon Blank Quantification for a Small-Sample High-Pressure Liquid Chromatography Purification Method.

    Science.gov (United States)

    Bour, Amy L; Walker, Brett D; Broek, Taylor A B; McCarthy, Matthew D

    2016-04-05

    Compound-specific radiocarbon analysis (CSRA) of amino acids (AAs) is of great interest as a proxy for organic nitrogen (N) cycling rates, dating archeological bone collagen, and investigating processes shaping the biogeochemistry of global N reservoirs. However, recoverable quantities of individual compounds from natural samples are often insufficient for radiocarbon ((14)C) analyses (quantification of C blanks (including sources, magnitudes, and variability) for a high-pressure liquid chromatography (HPLC) method designed to purify individual AAs from natural samples. We used pairs of AA standards with either modern (M) or dead (D) fraction modern (Fm) values to quantify MC and DC blanks within several chromatographic regions. Blanks were determined for both individual and mixed AA standard injections with peak loadings ranging from 10 to 85 μg C. We found 0.8 ± 0.4 μg of MC and 1.0 ± 0.5 μg of DC were introduced by downstream sample preparation (drying, combustion, and graphitization), which accounted for essentially the entire procedural blank for early eluting AAs. For late-eluting AAs, higher eluent organic content and fraction collected volumes contributed to total blanks of 1.5 ± 0.75 μg of MC and 3.0 ± 1.5 μg of DC. Our final measurement uncertainty for 20 μg of C of most AAs was ±0.02 Fm, although sample size requirements are larger for similar uncertainty in late-eluting AAs. These results demonstrate the first CSRA protocol for many protein AAs with uncertainties comparable to the lowest achieved in prior studies.

  3. Simultaneous quantification of 5 main components of Psoralea corylifolia L. in rats' plasma by utilizing ultra high pressure liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Gao, Qianqian; Xu, Zisheng; Zhao, Genhua; Wang, Heng; Weng, Zebin; Pei, Ke; Wu, Li; Cai, Baochang; Chen, Zhipeng; Li, Weidong

    2016-02-01

    Psoralea corylifolia L. has long been used in traditional Chinese medicine for treating and preventing many diseases. A group of flavonoid components are regarded as the active principals within the seeds. In this research, a rapid, accurate and sensitive ultra high pressure liquid chromatography tandem mass spectrometry (UHPLC/MS/MS) method has been established for simultaneous quantification of its 5 main components, namely, neobavaisoflavone, bavachin, isobavachalcone, bavachinin and corylifol A in rats' plasma after the rats were orally administrated with Buguzhi extract. Negative ion electrospray mode was applied in the detection process. Multiple reactions monitoring (MRM) mode was utilized for simultaneous quantitative analyzing of neobavaisoflavone (m/z 321.1→m/z 265.1), bavachin (m/z 323.1→m/z 119.0), isobavachalcone (m/z 323.2→m/z 119.0), bavachinin (m/z 337.2→m/z 119.0), corylifol A (m/z 389.2→m/z 277.0) and liquiritigenin (Internal Standard, m/z 255.1→m/z 119.0). Chromatographic separation of the above mentioned components was conducted on a Waters BEH-C18 column (100 mm×2.1mm, 1.7μm) with gradient elution system at flow rate of 0.3mL/min. The mobile phase was composed of acetonitrile and 0.1% formic acid solution. The lower limit of quantification (LLOQ) for each of the above analytes was 0.5ng/mL. Each of the analytes exhibited good linearity within the concentration range of 0.5-100ng/mL. The method was fully validated for its selectivity, accuracy, precision, stability, matrix effect and extraction recovery. The validated method has been successfully applied for simultaneous determination of the 5 flavonoids in rat plasma for the first time.

  4. High performance liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry for sensitive determination of bioactive amines in donkey milk.

    Science.gov (United States)

    La Torre, Giovanna Loredana; Saitta, Marcello; Giorgia Potortì, Angela; Di Bella, Giuseppa; Dugo, Giacomo

    2010-08-06

    In the present study we report on the optimization and validation of a sensitive high performance liquid chromatography atmospheric pressure chemical ionization mass spectrometry (HPLC-APCI-MS) method for the determination of 8 bioactive amines (histamine, tyramine, tryptamine, 2-phenylethylamine, cadaverine, putrescine, spermidine and spermine) in donkey milk samples. The method involves donkey milk pre-treatment to remove proteins and pre-column dansylation of the amines. HPLC in reversed phase mode has been used for bioactive amines separation and the operating condition of the APCI-MS system proved to be powerful and very efficient for peak assignment. The separation was accomplished in a short time with an excellent resolution for all the amine peaks. Quantification was carried out by monitoring the characteristic [M+H](+) ion of each amine derivative. The method sensitivity, linearity and repeatability were assayed with satisfactory results. The detection limits of the analysed amines ranged from 0.5 microg L(-1) to 15 microg L(-1); the highest LOD was for spermine. Also remarkably good recovery values were obtained; at the lowest spiking level (1 microg L(-1)) the percent mean recoveries ranged from 77.7 to 109.7. Furthermore, as the investigations relate to a complex matrix as donkey milk, suitable studies on matrix effect were performed. Finally, the developed and validated method was applied to analyse 13 donkey milk samples. Among the identified bioactive amines, putrescine, spermine and spermidine proved to be the main amines in donkey milk. Their concentration levels in the present study were lower than the values determined in mature human, cow and sow milk.

  5. Ultra-high-pressure liquid chromatography tandem mass spectrometry determination of antidepressant and anxiolytic drugs in neonatal meconium and maternal hair.

    Science.gov (United States)

    Pichini, Simona; Cortes, Laura; Marchei, Emilia; Solimini, Renata; Pacifici, Roberta; Gomez-Roig, Maria Dolores; García-Algar, Oscar

    2016-01-25

    A procedure based on ultra-high-pressure liquid chromatography tandem mass spectrometry has been developed for the determination of 22 antidepressant and anxiolytic drugs ad metabolites in the three consecutive maternal hair segments representing the pregnancy trimesters and paired neonatal meconium samples. After hair washing with methyl alcohol and diethyl ether and subsequent addition of internal standards, hair samples were treated with 500 μl VMA-T M3 reagent for 1h at 100 °C. After cooling, 100 μl M3 extract were diluted with 400 μl water and a volume of 10 μl was injected into chromatographic system. Meconium samples were firstly treated with 1 ml methyl alcohol and the organic layer back-extracted twice with 1.5 ml of a mixture of ethylacetate:hexane (80:20, v/v). Chromatographic separation was achieved at ambient temperature using a reverse-phase column and a linear gradient elution with two solvents: 0.3% formic acid in acetonitrile and 5mM ammonium formate pH 3. The mass spectrometer was operated in positive ion mode, using multiple reaction monitoring via positive electrospray ionization. The method was linear from the limit of quantification (0.05-1 ng/mg hair and 5-25 ng/g meconium depending on analyte under investigation;) to 10 ng/mg hair and 1000 ng/g meconium, with an intra- and inter-assay imprecision and inaccuracy always less than 20% and an analytical recovery between 66.6% and 95.3%, depending on the considered analyte and biological matrix. Using the validated method, 7 mothers were found positive to one or more hair segments and 5 meconium samples were found positive to one or more antidepressant and anxiolytic drugs, assessing prenatal exposure to these drugs following maternal consumption in one or more pregnancy trimesters.

  6. Ultra-high-pressure liquid chromatography tandem mass spectrometry determination of hallucinogenic drugs in hair of psychedelic plants and mushrooms consumers.

    Science.gov (United States)

    Pichini, Simona; Marchei, Emilia; García-Algar, Oscar; Gomez, Arelis; Di Giovannandrea, Rita; Pacifici, Roberta

    2014-11-01

    A procedure based on ultra-high-pressure liquid chromatography tandem mass spectrometry has been developed for the determination of mescaline, N,N-dimethyltryptamine, psilocin, psilocybin, salvinorin A in hair of consumers of psychedelic vegetal material such peyote or trichocereus cacti, psilocybe mushrooms, Salvia divinorum or psychedelic beverage ayahuasca. After hair washing with methyl alcohol and diethyl ether and subsequent addition of mescaline-d9 and 3,4-methylenedioxypropylamphetamine as internal standards, hair samples were treated with 250μl VMA-T M3 reagent for 1h at 100°C. After cooling, 100μl M3 extract were diluted with 400μl water and a volume of 10μl was injected into chromatographic system. Chromatographic separation was achieved at ambient temperature using a reverse-phase column and a linear gradient elution with two solvents: 0.3% formic acid in acetonitrile and 5mM ammonium formate pH 3. The mass spectrometer was operated in positive ion mode, using multiple reaction monitoring via positive electrospray ionization. The method was linear from the limit of quantification (0.03-0.05ng/mg depending on analyte under investigation) to 10ng/mg hair, with an intra- and inter-assay imprecision and inaccuracy always less than 15% and an analytical recovery between 79.6% and 97.4%, depending on the considered analyte. Using the validated method, mescaline was found in concentration range of 0.08-0.13ng/mg in hair of peyote smokers, 3.2ng salvinorin A per mg hair were determined in hair from a S. divinorum smoker, 5.6ng N,N-dimethyltryptamine per mg hair from an ayahuasca user and finally 0.8ng psilocybin per ng hair of a psilocybe consumer.

  7. Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

    Science.gov (United States)

    Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

    2015-12-01

    Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine.

  8. Atmospheric pressure chemical ionisation liquid chromatography/mass spectrometry of bacteriochlorophylls from Chlorobiaceae: characteristic fragmentations.

    Science.gov (United States)

    Airs, Ruth L; Keely, Brendan J

    2002-01-01

    Atmospheric pressure chemical ionisation liquid chromatography/mass spectrometry/mass spectrometry (APCI-LC/MS/MS) has been applied to the study of bacteriochlorophylls c, d, and e of phototrophic prokaryotes. Cultures of Chlorobiaceae containing bacteriochlorophyll c, d or e were examined using a high-resolution high-performance liquid chromatography (HPLC) method and APCI-LC/MS/MS employing post-column addition of formic acid. The results reveal complex distributions of bacteriochlorophyll homologues, with some closely eluting species giving isobaric protonated molecules. On-line LC/MS/MS studies reveal characteristic fragment ions for bacteriochlorophylls c, d, and e. Fragmentations involving loss of the extended alkyl substituents that are unique to bacteriochlorophylls c, d and e and their derivatives have been rationalised by studying the phaeophorbides and the results applied to the direct study of the bacteriochlorophylls.

  9. Analysis of Tocopherols by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    B. Edison

    2009-01-01

    Full Text Available : Gas chromatography is the key technique for organic components and also for tocopherols analysis. High performance liquid chromatography has an important role to take part in applications such as the handling of less usual samples, prevention of degradation of heat sensitive functional groups and for micro preparative purposes. Many approaches for development of improved methods are suggested, especially for reversed phase applications.

  10. High Performance Liquid Chromatography Experiments to Undergraduate Laboratories

    Science.gov (United States)

    Kissinger, Peter T.; And Others

    1977-01-01

    Reviews the principles of liquid chromatography with electrochemical detection (LCEC), an analytical technique that incorporates the advantages of both liquids chromatography and electrochemistry. Also suggests laboratory experiments using this technique. (MLH)

  11. Liquid Microjunction Surface Sampling Coupled with High-Pressure Liquid Chromatography-Electrospray Ionization-Mass Spectrometry for Analysis of Drugs and Metabolites in Whole-Body Thin Tissue Sections

    Energy Technology Data Exchange (ETDEWEB)

    Kertesz, Vilmos [ORNL; Van Berkel, Gary J [ORNL

    2010-01-01

    In this work, a commercially available autosampler was adapted to perform direct liquid microjunction (LMJ) surface sampling followed by a high-pressure liquid chromatography (HPLC) separation of the extract components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the utility of coupling a separation with this direct liquid extraction based surface sampling approach, four different organs (brain, lung, kidney, and liver) from whole-body thin tissue sections of propranolol dosed and control mice were examined. The parent drug was observed in the chromatograms of the surface sampling extracts from all the organs of the dosed mouse examined. In addition, two isomeric phase II metabolites of propranolol (an aliphatic and an aromatic hydroxypropranolol glucuronide) were observed in the chromatograms of the extracts from lung, kidney, and liver. Confirming the presence of one or the other or both of these glucuronides in the extract from the various organs was not possible without the separation. These drug and metabolite data obtained using the LMJ surface sampling/HPLC-MS method and the results achieved by analyzing similar samples by conventional extraction of the tissues and subsequent HPLC-MS analysis were consistent.

  12. Mallow carotenoids determined by high-performance liquid chromatography

    Science.gov (United States)

    Mallow (corchorus olitorius) is a green vegetable, which is widely consumed either fresh or dry by Middle East population. This study was carried out to determine the contents of major carotenoids quantitatively in mallow, by using a High Performance Liquid Chromatography (HPLC) equipped with a Bis...

  13. Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

    Science.gov (United States)

    DiNunzio, James E.

    1985-01-01

    Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

  14. Multichannel Detection in High-Performance Liquid Chromatography.

    Science.gov (United States)

    Miller, James C.; And Others

    1982-01-01

    A linear photodiode array is used as the photodetector element in a new ultraviolet-visible detection system for high-performance liquid chromatography (HPLC). Using a computer network, the system processes eight different chromatographic signals simultaneously in real-time and acquires spectra manually/automatically. Applications in fast HPLC…

  15. High-Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  16. Ultra high performance liquid chromatography of seized drugs

    NARCIS (Netherlands)

    Lurie, I.S.

    2010-01-01

    The primary goal of this thesis is to investigate the use of ultra high performance liquid chromatography (UHPLC) for the analysis of seized drugs. This goal was largely achieved and significant progress was made in achieving improved separation and detection of drugs of forensic interest.

  17. High-performance liquid chromatography with packed microchips

    OpenAIRE

    Ehlert, Steffen

    2011-01-01

    This work is explaining the importance of generating a densely packed chromatographic bed to achieve optimum separation efficiency in miniaturized liquid chromatography. The reduction of peak dispersion and enhancement of separation efficiency is the important problem in micro- and nano-separation that is to be solved to generate highly efficient chromatographic systems that can exploit all advantages of miniaturization. Therefore...

  18. Quantification of Tea Flavonoids by High Performance Liquid Chromatography

    Science.gov (United States)

    Freeman, Jessica D.; Niemeyer, Emily D.

    2008-01-01

    We have developed a laboratory experiment that uses high performance liquid chromatography (HPLC) to quantify flavonoid levels in a variety of commercial teas. Specifically, this experiment analyzes a group of flavonoids known as catechins, plant-derived polyphenolic compounds commonly found in many foods and beverages, including green and black…

  19. Simultaneous determination of triazines and their main transformation products in surface and urban wastewater by ultra-high-pressure liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Benvenuto, Federica; Marín, José M; Sancho, Juan V; Canobbio, Sergio; Mezzanotte, Valeria; Hernández, Félix

    2010-08-01

    This work describes the optimization, validation and application of an ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the quantification and confirmation of 11 compounds (atrazine, simazine, terbuthylazine, terbumeton, terbutryn and their main transformation products) in surface and wastewater samples. Several of these analytes are included in the list of priority substances in the framework on European Water Policy. The application of this method to water samples reveals that the most relevant transformation products (TPs) should be incorporated into current analytical methods to obtain a more realistic knowledge of water quality regarding pesticide contamination. TPs are generally more polar and mobile than parents and can be transported to the aquatic environment more easily than their precursors. This can explain their concentrations found in water, which in many cases are much higher than intact triazines. To efficiently combine UHPLC with MS/MS, a fast-acquisition triple quadrupole mass analyser was used. Working in selected reaction monitoring mode, up to three simultaneous transitions per compound were acquired, allowing a reliable quantification and confirmation at nanogram per litre levels. The method developed includes a pre-concentration step based on solid-phase extraction (OASIS HLB cartridges). Satisfactory recoveries (70-120%) and relative standard deviations (<20%) were obtained for all compounds in different water sample types spiked at two concentrations (0.025 and 0.1 microg/L in surface water; 0.25 and 1.0 microg/L in effluent wastewater; 0.5 and 2.0 microg/L in influent wastewater). The optimized method was found to have excellent sensitivity with instrumental detection limits as low as 0.03 pg. In addition, the influence of the matrix constituents on the ionization efficiency and the extraction recovery was studied in different types of Italian and Spanish surface and urban wastewater. Signal

  20. An improved method for retrospective quantification of sulfur mustard exposure by detection of its albumin adduct using ultra-high pressure liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Liu, ChangCai; Liang, LongHui; Xiang, Yu; Yu, HuiLan; Zhou, ShiKun; Xi, HaiLing; Liu, ShiLei; Liu, JingQuan

    2015-09-01

    Sulfur mustard (HD) adduct to human serum albumin (ALB) at Cys-34 residue has become an important and long-term retrospective biomarker of HD exposure. Here, a novel, sensitive, and convenient approach for retrospective quantification of HD concentration exposed to plasma was established by detection of the HD-ALB adduct using ultra-high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with a novel non-isotope internal standard (IS). The HD-ALB adduct was isolated from HD-exposed plasma with blue Sepharose. The adduct was digested with proteinase K to form sulfur-hydroxyethylthioethyl ([S-HETE])-Cys-Pro-Phe tripeptide biomarker. The tripeptide adduct could be directly analyzed by UHPLC-MS/MS without an additional solid phase extraction (SPE), which was considered as a critical procedure in previous methods. The easily available 2-chloroethyl ethylsulfide (2-CEES) as HD surrogate was first reported to be used as IS in place of traditional d8-HD for quantification of HD exposure. Furthermore, 2-CEES was also confirmed to be a good IS alternative for quantification of HD exposure by investigation of product ion spectra for their corresponding tripeptide adducts which exhibited identical MS/MS fragmentation behaviors. The method was found to be linear between 1.00 and 250 ng•mL(-1) HD exposure (R(2)>0.9989) with precision of <4.50% relative standard deviation (%RSD), accuracy range between 96.5% and 114%, and a calculated limit of detection (LOD) of 0.532 ng•mL(-1). The lowest reportable limit (LRL) is 1.00 ng•mL(-1), over seven times lower than that of the previous method. The entire method required only 0.1 mL of plasma sample and took under 7 h without special sample preparation equipment. It is proven to be a sensitive, simple, and rugged method, which is easily applied in international laboratories to improve the capabilities for the analysis of biomedical samples related to verification of the Chemical Weapon Convention (CWC).

  1. Determination of gemcitabine and its metabolite in human plasma using high-pressure liquid chromatography coupled with a diode array detector

    Institute of Scientific and Technical Information of China (English)

    Neng-ming LIN; Su ZENG; Sheng-lin MA; Yun FAN; Hai-jun ZHONG; Luo FANG

    2004-01-01

    AIM: To establish a high pressure liquid chromatography (HPLC) method for determination of the concentration of gemcitabine (dFdC) and its metabolite (dFdU) in human plasma. METHODS: Plasma 1.0mL spiked with floxuridine as an internal standard was extracted with 3.0 mL of methanol-acetonitrile (v/v, 1:9). The supernatant was evaporated at 60 ℃ and the residue was reconstituted with 0.5 mL of the solution used as the mobile phase. After centrifugation, 50 μL of the supernatant was injected into the HPLC system. Separation was achieved on a C18(4.6 mm×250 mm, 5μm) column at 25℃ with the flow rate of the mobile phase set to 0.8 mL/min. The compounds were detected at 268 nm. The mobile phase consisted of 40.0 mmol/L acetate ammonium buffer solution (pH 5.5) and acetonitrile (v/v, 97.5:2.5). RESULTS: The linear range was 0.20-10.0 mg/L (r=0.9999) for dFdC and 0.50-50.0 mg/L (r=0.9999) for dFdU. The limit of detection (LOD) was 0.10 mg/L for dFdC and 0.25mg/L for dFdU, while the limit of quantification (LOQ) was 0.20 mg/L (RSD<10%) for dFdC and 0.50 mg/L (RSD <3%) for dFdU. The average recovery of dFdC and dFdU by this method were 103.3% and 98.7%, respectively.For intra-day and inter-day, the corresponding standard deviations of the measurements of dFdC and dFdU were both less than 5.5%. CONCLUSION: An analytical method was established to measure the concentrations of dFdC and dFdU in human plasma and was effectively applied to the dFdC and dFdU pharmacokinetic studies of 8Chinese patients with malignant tumors.

  2. Quantitative analysis of acankoreoside A and acankoreagenin in the leaves of Schefflera octophylla and Schefflera actinophylla using pressurized liquid extraction and high-performance liquid chromatography coupled with evaporative light scattering detection.

    Science.gov (United States)

    Cao, Kai-Yue; Qiao, Chun-Feng; Zhao, Jing; Xie, Jing; Li, Shao-Ping

    2015-07-01

    A rapid method based on pressurized liquid extraction followed by high-performance liquid chromatography coupled with evaporative light scattering detection was firstly developed for the quantitative analysis of two bioactive triterpenoids (acankoreoside A and acankoreagenin) in the leaves of Schefflera octophylla and Schefflera actinophylla. The analysis was performed on an Agilent Zorbax SB-Aq column (4.6 × 50 mm, 3.5 μm) with gradient elution of 0.1% formic acid and acetonitrile. Calibration curves of two analytes showed good linearity (R(2) > 0.9990) within the tested ranges. This novel method is simple, rapid and accurate, and the results of quantification showed that contents of each investigated compound is significant high in natural S. octophylla (6.36-14.83%), which indicated that natural S. octophylla as potential medicinal resource. Furthermore, hierarchical clustering analysis based on the typical peaks of acankoreoside A and acankoreagenin from the 17 tested samples showed that natural and cultured Schefflera species were in different clusters, which could provide a means of discriminating between Schefflera species from different origins. Thus, acankoreoside A and acankoreagnin could be selected markers for quality control of S. octophylla and S. actinophylla.

  3. Influence of pressure and temperature on the physico-chemical properties of mobile phase mixtures commonly used in high-performance liquid chromatography.

    Science.gov (United States)

    Billen, Jeroen; Broeckhoven, Ken; Liekens, Anuschka; Choikhet, Konstantin; Rozing, Gerard; Desmet, Gert

    2008-11-07

    To fulfil the increasing demand for faster and more complex separations, modern HPLC separations are performed at ever higher pressures and temperatures. Under these operating conditions, it is no longer possible to safely assume the mobile phase fluid properties to be invariable of the governing pressures and temperatures, without this resulting in significantly deficient results. A detailed insight in the influence of pressure and temperature on the physico-chemical properties of the most commonly used liquid mobile phases: water-methanol and water-acetonitrile mixtures, therefore becomes very timely. Viscosity, isothermal compressibility and density were measured for pressures up to 1000 bar and temperatures up to 100 degrees C for the entire range of water-methanol and water-acetonitrile mixtures. The paper reports on two different viscosity values: apparent and real viscosities. The apparent viscosities represent the apparent flow resistance under high pressure referred to by the flow rates measured at atmospheric pressure. They are of great practical use, because the flow rates at atmospheric pressure are commonly stable and more easily measurable in a chromatographic setup. The real viscosities are those complying with the physical definition of viscosity and they are important from a fundamental point of view. By measuring the isothermal compressibility, the actual volumetric flow rates at elevated pressures and temperatures can be calculated. The viscosities corresponding to these flow rates are the real viscosities of the solvent under the given elevated pressure and temperature. The measurements agree very well with existing literature data, which mainly focus on pure water, methanol and acetonitrile and are only available for a limited range of temperatures and pressures. As a consequence, the physico-chemical properties reported on in this paper provide a significant extension to the range of data available, hereby providing useful data to practical as

  4. Application of a radioactivity detector to the analysis of /sup 14/C-Carmoisine metabolites by ion-pair high-pressure liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Tragni, E.; Costa, L.G.; Marinovich, M.; Galli, C.L.

    1984-04-01

    /sup 14/C-Carmoisine was incubated under anaerobic conditions with a suspension of human feces. Analyses of the incubation medium by high-performance liquid chromatography (HPLC) attached to a radioactivity monitor (RAM) showed the same radioactivity profile as the urine and feces of rats dosed with the same azodye (200 mg kg-1; 25 microCi). The analyses were carried out with a 5 micron RP-C18 chromatographic column, using a linear gradient profile of different concentrations of water, methanol and an ion-pair reagent. Five radioactive peaks were present in the radiochromatogram , in addition to unmodified Carmoisine. The major peak retained half of the specific activity of Carmoisine, and exhibited the retention time and the u.v. spectrum of authentic naphthionic acid. The results demonstrate the value and the advantage of using the in vitro preparation as a model to detect and to identify the metabolites of similar synthetic azodyes used as food additives.

  5. Ergot alkaloids in rye flour determined by solid-phase cation-exchange and high-pressure liquid chromatography with fluorescence detection

    DEFF Research Database (Denmark)

    Storm, Ida Marie Lindhardt Drejer; Rasmussen, Peter Have; Strobel, B.W.

    2008-01-01

    Ergot alkaloids are mycotoxins that are undesirable contaminants of cereal products, particularly rye. A method was developed employing clean-up by cation-exchange solid-phase extraction, separation by high-performance liquid chromatography under alkaline conditions and fluorescence detection....... It is capable of separating and quantifying both C8-isomers of ergocornine, alpha-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61% +/- 10% with limits of detection from 0.2 to 1.1 mu g kg(-1). Twenty-four unknown rye flour samples from Danish mills contained on average 46 mu...... g kg(-1) with a maximum content of 234 mu g kg(-1). The most common ergot alkaloids were ergotamine and alpha-ergocryptine including their C8-isomers. A total of 54% of the ergot alkaloids were detected as C(8)-S isomers....

  6. Determination of ethylenethiourea (ETU) and propylenethiourea (PTU) in foods by high performance liquid chromatography-atmospheric pressure chemical ionisation-medium-resolution mass spectrometry.

    Science.gov (United States)

    Startin, James R; Hird, Simon J; Sykes, Mark D

    2005-03-01

    A robust and sensitive method for the determination of ethylenethiourea (ETU) and iso-propylenethiourea (i-PTU) in foods is reported. ETU and i-PTU were extracted by blending with dichloromethane (DCM) in the presence of sodium sulphate, sodium carbonate, thiourea and ascorbic acid. 2H4-ETU and n-PTU were used as internal standards. After filtration the DCM was removed by rotary evaporation and the extract re-dissolved in water before analysis by reversed-phase liquid chromatography with detection by atmospheric pressure chemical ionization-mass spectrometry using a double focusing mass spectrometer at a resolution of 5000. Mean recoveries of ETU and i-PTU from fruit-based, cereal-based and meat-based infant foods, potato chips and tinned potatos at 0.01 mg kg(-1) and from pizza and yoghurt at 0.02-0.1 mg kg(-1) were 95% and 97% respectively. Precision, including both repeatability and internal reproducibility, was in the range of 3.1-13.1%.

  7. Parallel ultra high pressure liquid chromatography-mass spectrometry for the quantification of HIV protease inhibitors using dried spot sample collection format.

    Science.gov (United States)

    Watanabe, Kyoko; Varesio, Emmanuel; Hopfgartner, Gérard

    2014-08-15

    An assay was developed and validated for the quantification of eight protease inhibitors (indinavir (IDV), ritonavir (RTV), lopinavir (LPV), saquinavir (SQV), amprenavir (APV), nelfinavir (NFV), atazanavir (AZV) and darunavir (DRV)) in dried plasma spots using parallel ultra-high performance liquid chromatography and mass spectrometry detection in the multiple reaction monitoring mode. For each analyte an isotopically labeled internal standard was used and the assay based on liquid-solid extraction the area response ratio (analyte/IS) was found to be linear; from 0.025 μg/ml to 20 μg/ml for IDV, SQV, DRV, AZV, LPV, from 0.025 μg/ml to 10 μg/ml for NFV, APV and from 0.025 μg/ml to 5 μg/ml for RTV using 15 μl of plasma spotted on filter paper placed in a sample tube. The total analysis time was of 4 min and inter-assay accuracies and precisions were in the range of 87.7-109% and 2.5-11.8%, respectively. On dried plasma spots all analytes were found to be stable for at least 7 days. Practicability of the assay to blood was also demonstrated. The sample drying process could be reduced to 5 min using a commercial microwave system without any analyte degradation. Together with quantification, confirmatory analysis was performed on representative clinical samples.

  8. Analysis of Free Fatty Acids on the Fingertips by High Performance Liquid Chromatography.

    Science.gov (United States)

    1978-12-20

    This investigation studied the efficiency of high performance liquid chromatography in the determination of free fatty acids present on the...utilized to eliminate the microbial contamination. The high performance liquid chromatography provided excellent separation of skin fatty acids for

  9. Quantitative separation of tetralin hydroperoxide from its decomposition products by high performance liquid chromatography

    Science.gov (United States)

    Worstell, J. H.; Daniel, S. R.

    1981-01-01

    A method for the separation and analysis of tetralin hydroperoxide and its decomposition products by high pressure liquid chromatography has been developed. Elution with a single, mixed solvent from a micron-Porasil column was employed. Constant response factors (internal standard method) over large concentration ranges and reproducible retention parameters are reported.

  10. Determination of a Jet Fuel Metal Deactivator by High Performance Liquid Chromatography

    Science.gov (United States)

    1983-06-01

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY Paul C. Hayes, Jr. Fuels Branch...SUPPLEMENTARY NOTES 19. KEY WORDS (Continue on reverse side if necessary and identify by block number) High Performance Liquid Chromatography absorbance...SYMBOL HPLC High Performance Liquid Chromatography P-4 jet propulsion fuel, wide-boiling range, conforming to MIL-T-5624L MDA metal deactivator,

  11. Determination of Stabiliser Contents in Advanced Gun Propellants by Reverse Phase High Performance Liquid Chromatography

    Science.gov (United States)

    1994-03-01

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY N"m A.R. TURNER AND A. WHITE...TO biEPROOU.; AND SELL THIS REPORT Determination of Stabiliser Contents in Advanced Gun Propellants by Reverse Phase High Performance Liquid Chromatography A.R...8217/......... .. Availability Cooes Dist Avaiardlo A-i Determination of Stabiliser Contents in Advanced Gun Propellants by Reverse Phase High Performance Liquid Chromatography

  12. Temperature-Modulated Array High-Performance Liquid Chromatography

    OpenAIRE

    Premstaller, Andreas; Xiao, Wenzhong; Oberacher, Herbert; O'Keefe, Matthew; Stern, David; Willis, Thomas; Huber, Christian G.; Peter J. Oefner

    2001-01-01

    Using novel monolithic poly(styrene-divinylbenzene) capillary columns with an internal diameter of 0.2 mm, we demonstrate for the first time the feasibility of constructing high-performance liquid chromatography arrays for the detection of mutations by heteroduplex analysis under partially denaturing conditions. In one embodiment, such an array can be used to analyze one sample simultaneously at different temperatures to maximize the detection of mutations in DNA fragments containing multiple...

  13. Determination of aminocresol isomers by high-speed liquid chromatography.

    Science.gov (United States)

    Sakurai, H; Kito, M

    Aminocresol isomers (4-hydroxy-m-toluidine [II], 3-hydroxy-p-toluidine [II], 2-hydroxy-p-toluidine [III]) and p-aminophenol have been separated and determined by a high-speed liquid Chromatographie method. Since this method is applicable in aqueous media, it was used to investigate the suitability of a haemin-cysteine system as a model for the cytochrome P-450 mono-oxygenase system, by determination of the [I], [II], [III] and p-aminophenol formed.

  14. Characterization of typical chemical background interferences in atmospheric pressure ionization liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Guo, Xinghua; Bruins, Andries P.; Covey, Thomas R.

    2006-01-01

    The structures and origins of typical chemical background noise ions in positive atmospheric pressure ionization liquid chromatography/mass spectrometry (API LC/MS) are investigated and summarized in this study. This was done by classifying chemical background ions using precursor and product ion sc

  15. Ultrasonic Propagation in Liquids Under High Pressures

    Science.gov (United States)

    1948-12-01

    34 Proc. Am, Acad. Arts Sci. 19, 143 (1923). 28. Bridgman P. W., "The Viscosity of Liquids under Pressure," Proc. Nat. Acad. Sci. 119 603 (1925). TM3...1932). 42. Ewell, R. H., and Eyring, H., "Theory of the Viscosity of Liquids as a Function of Temperature and Pressureg" J. Chem. Phys. 1, 726 (1937

  16. Simultaneous determination of acetylsalicylic acid and salicylic acid in human plasma by isocratic high-pressure liquid chromatography with post-column hydrolysis and fluorescence detection.

    Science.gov (United States)

    Hobl, Eva-Luise; Jilma, Bernd; Ebner, Josef; Schmid, Rainer W

    2013-06-01

    A selective, sensitive and rapid high-performance liquid chromatography method with post-column hydrolysis and fluorescence detection was developed for the simultaneous quantification of acetylsalicylic acid and its metabolite salicylic acid in human plasma. Following the addition of 2-hydroxy-3-methoxybenzoic acid as internal standard and simple protein precipitation with acetonitrile, the analytes were separated on a ProntoSIL 120 C18 ace-EPS column (150 × 2 mm, 3 µm) protected by a C8 guard column (5 µm). The mobile phase, 10 mm formic acid in water (pH 2.9) and acetonitrile (70:30, v/v), was used at a flow rate of 0.35 mL/min. After on-line post-column hydrolysis of acetylsalicylic acid (ASA) to salicylic acid (SA) by addition of alkaline solution, the analytes were measured at 290 nm (λex ) and 400 nm (λem ). The method was linear in the concentration ranges between 0.05 and 20 ng/μL for both ASA and SA with a lower limit of quantification of 25 pg/μL for SA and 50 pg/μL for ASA. The limit of detection was 15 pg/μL for SA and 32.5 pg/μL for ASA. The analysis of ASA and SA can be carried out within 8 min; therefore this method is suitable for measuring plasma concentrations of salicylates in clinical routine.

  17. A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

    2016-06-01

    In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples.

  18. Wipe selection for the analysis of surface materials containing chemical warfare agent nitrogen mustard degradation products by ultra-high pressure liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Willison, Stuart A

    2012-12-28

    Degradation products arising from nitrogen mustard chemical warfare agent were deposited on common urban surfaces and determined via surface wiping, wipe extraction, and liquid chromatography–tandem mass spectrometry detection. Wipes investigated included cotton gauze, glass fiber filter, non-woven polyester fiber and filter paper, and surfaces included several porous (vinyl tile, painted drywall, wood) and mostly non-porous (laminate, galvanized steel, glass) surfaces. Wipe extracts were analyzed by ultra-high pressure liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) and compared with high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) results. An evaluation of both techniques suggests UPLC–MS/MS provides a quick and sensitive analysis of targeted degradation products in addition to being nearly four times faster than a single HPLC run, allowing for greater throughput during a wide-spread release concerning large-scale contamination and subsequent remediation events. Based on the overall performance of all tested wipes, filter paper wipes were selected over other wipes because they did not contain interferences or native species (TEA and DEA) associated with the target analytes, resulting in high percent recoveries and low background levels during sample analysis. Other wipes, including cotton gauze, would require a pre-cleaning step due to the presence of large quantities of native species or interferences of the targeted analytes. Percent recoveries obtained from a laminate surface were 47–99% for all nitrogen mustard degradation products. The resulting detection limits achieved from wipes were 0.2 ng/cm(2) for triethanolamine (TEA), 0.03 ng/cm(2) for N-ethyldiethanolamine (EDEA), 0.1 ng/cm(2) for N-methyldiethanolamine (MDEA), and 0.1 ng/cm(2) for diethanolamine (DEA).

  19. Use of high pressure liquid chromatography to study chemically induced alterations in the pattern of benzo(a)pyrene metabolism. [Rat liver microsomes

    Energy Technology Data Exchange (ETDEWEB)

    Freudenthal, R.I.; Leber, A.P.; Emmerling, D.; Clarke, P.

    1975-11-01

    The metabolism of radiolabeled benzo(a)pyrene (BP) by control, 3-methylcholanthrene (3-MC) induced and 1,1,1-trichloropropene-2,3-oxide (TCPO)-inhibited rat liver microsomes was measured using fluorescence, radiometric, and high-pressure liquid chromatographic (HPLC) assays. Significant differences in the total measurable metabolism of BP by the three microsomal enzyme incubations resulted from the use of the three assay procedures. Appreciable differences in the concentration of the metabolite fractions after 3-MC induction and TCPO inhibition are clearly demonstrated. NMR analysis revealed that while the 3-hydroxy-BP fraction is greater than 90 percent pure, the 9-hydroxy fraction contains a number of metabolites having essentially identical retention times.

  20. Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    González-Curbelo, Miguel Ángel; Lehotay, Steven J; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

    2014-09-01

    The "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) approach to sample preparation is widely applied in pesticide residue analysis, but the use of magnesium sulfate and other nonvolatile compounds for salting out in the method is not ideal for mass spectrometry. In this study, we developed and evaluated three new different versions of the QuEChERS method using more volatile salts (ammonium chloride and ammonium formate and acetate buffers) to induce phase separation and extraction of 43 representative pesticide analytes of different classes. Fast low-pressure gas chromatography tandem mass spectrometry (LPGC-MS/MS) and liquid chromatography (LC)-MS/MS were used for analysis. The QuEChERS AOAC Official Method 2007.01 was also tested for comparison purposes. Of the studied methods, formate buffering using 7.5g of ammonium formate and 15mL of 5% (v/v) formic acid in acetonitrile for the extraction of 15g of sample (5g for wheat grain) provided the best performance and practical considerations. Method validation was carried out with and without the use of dispersive solid-phase extraction for cleanup, and no significant differences were observed for the majority of pesticides. The method was demonstrated in quantitative analysis for GC- and LC-amenable pesticides in 4 representative food matrices (apple, lemon, lettuce, and wheat grain). With the typical exceptions of certain pH-dependent and labile pesticides, 90-110% recoveries and food applications.

  1. Monitoring stevioside in soju by high-performance liquid chromatography and liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Ni, Fan; Ammann, Jeffrey; Mabud, Abdul

    2007-01-01

    A method using high-performance liquid chromatography (HPLC) with UV absorption detection was developed to monitor stevioside in soju, a distilled spirits product that is commercially available. The method uses a single-step dilution for sample preparation. It completely eliminates the time-consuming process of solid-phase extraction. A method using HPLC/mass spectrometry was optimized to confirm the identities of stevioside and other related impurities, including rebaudioside A, rebaudioside C, and dulcoside. The method was validated. The validation parameters included range (10.1-1007.3 ppm), precision, linearity, accuracy, robustness, system suitability, and intermediate precision. Stevioside standard solutions at 6 concentration levels were prepared for the validation work, including the tests for precision, linearity, and accuracy. The solutions were prepared in triplicate for each concentration. The relative standard deviation for the precision test was 0.999. The average recovery ranged from 95.7 to 101.1% for the soju samples spiked with stevioside standard. The detection limit for stevioside was estimated at 75 ppb. The method was used to screen several soju samples; no detectable stevioside was found in the samples.

  2. Quantification of tryptophan in plasma by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Renata Romanholi Pinhati

    2012-01-01

    Full Text Available A simple, rapid and selective method using high-performance liquid chromatography with ultraviolet detection (267 nm was applied for the determination of tryptophan in plasma. Separation was carried out on a C18 column (150 x 4.6 mm internal diameter in 6 min. The mobile phase consisted of 5 mM the sodium acetate and acetonitrile (92:8, v/v. The method was shown to be precise and accurate, and good recovery of analyte was achieved, characterizing the method as efficient and reliable for use in laboratory analysis.

  3. High Performance Liquid Chromatography of Vitamin A: A Quantitative Determination.

    Science.gov (United States)

    Bohman, Ove; And Others

    1982-01-01

    Experimental procedures are provided for the quantitative determination of Vitamin A (retinol) in food products by analytical liquid chromatography. Standard addition and calibration curve extraction methods are outlined. (SK)

  4. Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 column(4.6 mm×250 mm,5 μm)was used with a mobile phase of 0.02 M potassium dihydrogen phosphate buffer(pH 6.0)-methanol(92∶8)at a flow rate of 1.0 mL/min,and UV detector set at 254 nm was used for monitoring the eluents.Results The method was simple,rapid,selective and capable of separating all r...

  5. Temperature-controlled ionic liquid dispersive liquid phase microextraction combined with ultra-high-pressure liquid chromatography for the rapid determination of triclosan,triclocarban and methyl-triclosan in aqueous samples

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    As extraction solvents,ionic liquids have green characteristics.In this study,an environmentally benign analytical method termed temperature-controlled ionic liquid dispersive liquid phase microextraction (TIL-DLME) combined with ultra-highpressure liquid chromatography (UHPLC)-tunable ultraviolet detection (TUV) was developed for the pre-concentration and determination of triclosan (TCS),triclocarban (TCC) and methyl-triclosan (M-TCS) in water samples.Significant parameters that may affect extraction efficiencies were examined and optimized,including the types and amount of ionic liquids,volume of the diluent,heating temperature,cooling time,salt effect and pH value.Under the optimum conditions,linearity of the method was observed in the ranges of 0.0100-100 μgL-1 for TCS and M-TCS,and 0.00500-50.0 μgL-1 for TCC with correlation coefficients (r2) > 0.9903.The limits of detection (LODs) ranged from 1.15 to 5.33 ngL-1.TCS in domestic water and TCC in reclaimed water were detected at the concentrations of 1.01 and 0.126 μgL-1,respectively.The spiked recoveries of the three target compounds in reclaimed water,irrigating water,waste water and domestic water samples were obtained in the ranges of 68.4%-71.9%,61.6%-87.8%,58.9%-74.9% and 64.9%-92.4%,respectively.Compared with the previous dispersive liquid-liquid microextraction method (DLLME) about the determination of TCS,TCC and M-TCS,this method is not only more environmentally friendly but also more sensitive.

  6. Principles of Liquid Chromatography

    Science.gov (United States)

    Bakalyar, Stephen R.

    This article reviews the basic principles of high performance liquid chromatography (HPLC). The introductory section provides an overview of the HPLC technique, placing it in historical context and discussing the elementary facts of the separation mechanism. The next section discusses the nature of resolution, describing the two principal aspects, zone center separation and zone spreading. The third section takes a detailed look at how HPLC is used in practice to achieve a separation. It discusses the three key variables that need to be adjusted: retention, efficiency, and selectivity. A fourth section is concerned with various relationships of practical importance: flow rate, temperature, and pressure. A final section discusses future trends in HPLC.

  7. Simultaneous determination of 13 carotenoids by a simple C18 column-based ultra-high-pressure liquid chromatography method for carotenoid profiling in the astaxanthin-accumulating Haematococcus pluvialis.

    Science.gov (United States)

    Jin, Hui; Lao, Yong Min; Zhou, Jin; Zhang, Huai Jin; Cai, Zhong Hua

    2017-03-10

    A simple ultra-high-pressure liquid chromatography (UHPLC) method for rapidly and simultaneously identifying thirteen carotenoids in Haematococcus pluvialis was developed in this study. The method is capable of effectively separating two astaxanthin isomers, two ζ-carotene isomers, and three phytoene isomers on two simple C18 columns within 9 and 12min only by using methanol and acetonitrile, respectively. To our best knowledge, this is the rapidest method for these carotenoid isomers, currently. Using this method, carotenoid profiling in the astaxanthin-accumulating H. pluvialis under environmental stresses was successfully carried out. Results indicated that carotenoid biosynthesis was differentially perturbed by environmental stresses, indicating that this simple and rapid method is suitable to not only bacterial but also algal samples, with potential applications for a wide range of samples from plant to animal. Finally, possible reasons for the elution order of carotenoids were studied.

  8. Method development for the determination of 24S-hydroxycholesterol in human plasma without derivatization by high-performance liquid chromatography with tandem mass spectrometry in atmospheric pressure chemical ionization mode.

    Science.gov (United States)

    Sugimoto, Hiroshi; Kakehi, Masaaki; Satomi, Yoshinori; Kamiguchi, Hidenori; Jinno, Fumihiro

    2015-10-01

    We developed a highly sensitive and specific high-performance liquid chromatography with tandem mass spectrometry method with an atmospheric pressure chemical ionization interface to determine 24S-hydroxycholesterol, a major metabolite of cholesterol formed by cytochrome P450 family 46A1, in human plasma without any derivatization step. Phosphate buffered saline including 1% Tween 80 was used as the surrogate matrix for preparation of calibration curves and quality control samples. The saponification process to convert esterified 24S-hydroxycholesterol to free sterols was optimized, followed by liquid-liquid extraction using hexane. Chromatographic separation of 24S-hydroxycholesterol from other isobaric endogenous oxysterols was successfully achieved with gradient mobile phase comprised of 0.1% propionic acid and acetonitrile using L-column2 ODS (2 μm, 2.1 mm id × 150 mm). This assay was capable of determining 24S-hydroxycholesterol in human plasma (200 μL) ranging from 1 to 100 ng/mL with acceptable intra- and inter-day precision and accuracy. The potential risk of in vitro formation of 24S-hydroxycholesterol by oxidation from endogenous cholesterol in human plasma was found to be negligible. The stability of 24S-hydroxycholesterol in relevant solvents and human plasma was confirmed. This method was successfully applied to quantify the plasma concentrations of 24S-hydroxycholesterol in male and female volunteers.

  9. Analytical capabilities of high performance liquid chromatography - Atmospheric pressure photoionization - Orbitrap mass spectrometry (HPLC-APPI-Orbitrap-MS) for the trace determination of novel and emerging flame retardants in fish.

    Science.gov (United States)

    Zacs, D; Bartkevics, V

    2015-10-22

    A new analytical method was established and validated for the analysis of 27 brominated flame retardants (BFRs), including so called "emerging" and "novel" BFRs (EBFRs and NBFRs) in fish samples. High performance liquid chromatography (HPLC) coupled to Orbitrap mass spectrometry (Orbitrap-MS) employing atmospheric pressure photoionization (APPI) interface operated in negative mode was used for the identification/quantitation of contaminants. HPLC-Orbitrap-MS analysis provided a fast separation of selected analytes within 14 min, thus demonstrating a high throughput processing of samples. The developed methodology was tested by intralaboratory validation in terms of recovery, repeatability, linear calibration ranges, instrumental and method limits of quantitation (i-LOQ and m-LOQ), and where possible, trueness was verified by analysis of certified reference materials (CRMs). Recoveries of analytes were between 80 and 119%, while the repeatability in terms of relative standard deviations (RSDs) was in the range from 1.2 to 15.5%. The measured values for both analyzed CRMs agreed with the provided consensus values, revealing the recovery of reference concentrations in 72-119% range. The elaborated method met the sensitivity criterion according to Commission Recommendation 2014/118/EU on monitoring of BFRs in food products for majority of the compounds. The concentrations of polybrominated diphenyl ethers (PBDEs) in real samples determined by HPLC-APPI-Orbitrap-MS method and validated gas chromatography-high-resolution mass spectrometry (GC-HRMS) method were found to be in a good agreement.

  10. Atmospheric pressure photoionisation : An ionization method for liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Robb, DB; Covey, TR; Bruins, AP

    2000-01-01

    Atmospheric pressure photoionization (APPI) has been successfully demonstrated to provide high sensitivity to LC-MS analysis. A vacuum-ultraviolet lamp designed for photoionization detection in gas chromatography is used as a source of 10-eV photons. The mixture of samples and solvent eluting from a

  11. Towards Chip Scale Liquid Chromatography and High Throughput Immunosensing

    Energy Technology Data Exchange (ETDEWEB)

    Ni, Jing [Iowa State Univ., Ames, IA (United States)

    2000-09-21

    This work describes several research projects aimed towards developing new instruments and novel methods for high throughput chemical and biological analysis. Approaches are taken in two directions. The first direction takes advantage of well-established semiconductor fabrication techniques and applies them to miniaturize instruments that are workhorses in analytical laboratories. Specifically, the first part of this work focused on the development of micropumps and microvalves for controlled fluid delivery. The mechanism of these micropumps and microvalves relies on the electrochemically-induced surface tension change at a mercury/electrolyte interface. A miniaturized flow injection analysis device was integrated and flow injection analyses were demonstrated. In the second part of this work, microfluidic chips were also designed, fabricated, and tested. Separations of two fluorescent dyes were demonstrated in microfabricated channels, based on an open-tubular liquid chromatography (OT LC) or an electrochemically-modulated liquid chromatography (EMLC) format. A reduction in instrument size can potentially increase analysis speed, and allow exceedingly small amounts of sample to be analyzed under diverse separation conditions. The second direction explores the surface enhanced Raman spectroscopy (SERS) as a signal transduction method for immunoassay analysis. It takes advantage of the improved detection sensitivity as a result of surface enhancement on colloidal gold, the narrow width of Raman band, and the stability of Raman scattering signals to distinguish several different species simultaneously without exploiting spatially-separated addresses on a biochip. By labeling gold nanoparticles with different Raman reporters in conjunction with different detection antibodies, a simultaneous detection of a dual-analyte immunoassay was demonstrated. Using this scheme for quantitative analysis was also studied and preliminary dose-response curves from an immunoassay of a

  12. Determination of 21-hydroxydeflazacort in human plasma by high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry. Application to bioequivalence study.

    Science.gov (United States)

    Ifa, D R; Moraes, M E; Moraes, M O; Santagada, V; Caliendo, G; de Nucci, G

    2000-03-01

    A liquid chromatographic atmospheric pressure chemical ionization tandem mass spectrometric method is described for the determination of 21-hydroxydeflazacort in human plasma using dexamethasone 21-acetate as an internal standard. The procedure requires a single diethyl ether extraction. After evaporation of the solvent under a nitrogen flow, the analytes are reconstituted in the mobile phase, chromatographed on a C18 reversed-phase column and analyzed by mass spectrometry via a heated nebulizer interface where they are detected by multiple reaction monitoring. The method has a chromatographic run time of less than 5 min and a linear calibration curve with a range of 1-400 ng ml(-1) (r>0.999). The between-run precision, based on the relative standard deviation for replicate quality controls, was Comercio, Brazil, as a test formulation, and Calcort from Merrell Lepetit, Brazil, as a reference formulation) in 24 healthy volunteers of both sexes who received a single 30 mg dose of each formulation. The study was conducted using an open, randomized, two-period crossover design with a 7-day washout interval. The 90% confidence interval (CI) of the individual geometric mean ratio for Denacen/Calcort was 89.8-109.5% for area under the curve AUC(0-24 h) and 80.7-98.5% for Cmax. Since both the 90% CI for AUC(0-24 h) and Cmax were included in the 80-125% interval proposed by the US Food and Drug Administration, Denacen was considered bioequivalent to Calcort according to both the rate and extent of absorption.

  13. Optimized determination of polybrominated diphenyl ethers by ultrasound-assisted liquid-liquid extraction and high-performance liquid chromatography.

    Science.gov (United States)

    He, Kuang; Lv, YuanCai; Chen, YuanCai

    2014-10-01

    A method based on ultrasound-assisted liquid-liquid extraction and high-performance liquid chromatography has been optimized for the determination of six polybrominated diphenyl ether congeners. The optimal condition relevant to the extraction was first investigated, more than 98.7 ± 0.7% recovery was achieved with dichloromethane as extractant, 5 min extraction time, and three cycles of ultrasound-assisted liquid-liquid extraction. Then multiple function was employed to optimize polybrominated diphenyl ether detection conditions with overall resolution and chromatography signal area as the responses. The condition chosen in this experiment was methanol/water 93:7 v/v, flow rate 0.80 mL/min, column temperature 30.0°C. The optimized technique revealed good linearity (R(2) > 0.9962 over a concentration range of 1-100 μg/L) and repeatability (relative standard deviation liquid-liquid extraction coupled with high-performance liquid chromatography was effective to identify and quantify the complex polybrominated diphenyl ethers in effluent samples.

  14. Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry.

    Science.gov (United States)

    Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca

    2016-01-08

    This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1. Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSDdairy products studied. The proposed method improves the performance of AFM1 analysis in milk samples as AFM1 determination is performed with a degree of accuracy higher than the conventional methods. Other advantages are the reduction of sample preparation procedure, time and cost of the analysis, enabling high sample throughput that meet the current concerns of food safety and the public health protection.

  15. Detection of flunixin in equine urine using high-performance liquid chromatography with particle beam and atmospheric pressure ionization mass spectrometry after solid-phase extraction.

    Science.gov (United States)

    Stanley, S M; Owens, N A; Rodgers, J P

    1995-05-05

    A normal-phase HPLC method combined with particle-beam mass spectrometry (PB-MS) was developed for the analysis of non-steroidal anti-inflammatory drugs (NSAIDs). The forty one NSAIDs analysed responded in one or more (electron impact, positive and negative chemical ionisation) modes and highly characteristic spectra were produced. A mixed-mode solid-phase extraction (SPE) method for isolating acidic NSAIDs was developed using the Bond Elut Certify II cartridge. The average recovery was 88.5%. Flunixin, extracted by SPE from urine of a mare to which the meglumine salt had been administered was positively identified by HPLC-PB-MS and HPLC-atmospheric pressure ionization (API) MS methods.

  16. 植物花青苷液质联用方法的分析鉴定%Golden rules of separation and characterization of plant anthocyanins by high pressure liquid chromatography-tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    张洁; 李崇晖; 王亮生; 陈峰

    2013-01-01

      花青苷(anthocyanins)是植物中广泛存在的水溶性色素,在食品加工业中具有重要的地位。花青苷与人体健康密切相关,具有较强的抗氧化、抗炎症、抗微生物、抑制血小板凝聚和抗肿瘤等功效,已作为重要的功能因子而受到广泛的关注。花青苷成分的分析鉴定是花青苷生物活性研究的基础。然而,花青苷种类繁多,结构修饰多样,同时易受环境条件的影响,难以分离鉴定。高压液相色谱-二极管阵列检测-质谱联用技术(HPLC-DAD-MS)是花青苷分析最常规的手段。本文综述了如何利用HPLC-DAD-MS快速有效分离花青苷以及结构解析的一般规律及经验,以期为高附加值资源筛选以及花青苷构效关系的进一步揭示提供重要的化学基础。%  Anthocyanins are important water-soluble pigments, which have significant influence in food processing industry. Anthocyanins have anti-oxidant, anti-inflammatory, anti-antimicrobial, inhibition of platelet aggregation and anticancer activity, and have been the focus as important functional ingredients. Separation and identification of anthocyanins are the base for studying their bioactive effects. However, the complexity and va-riety of anthocyanins make it difficult to characterize the composition of anthocyanins. High pressure liquid chromatography (HPLC) coupled with mass spectrometry has become the standard and most powerful method for routine anthocyanin analysis. This paper reviewed the golden rules for separation and identification of anthocya-nins by high pressure liquid chromatography-tandem mass spectrometry (HPLC-DAD-MS), which might provide the chemical evidence for clarification of structure-activity relationship and screening for high value-added re-sources.

  17. A Generalized Equation of State for High-Pressure Liquids

    Institute of Scientific and Technical Information of China (English)

    LIANG Yan-bo; TONG Jing-shan

    2005-01-01

    An equation of state (EOS) for high-pressure liquids, I.e., Tait EOS, is deduced according to isothermal compressibility KT=-1/V·((а)V/(а)p)T·.Based on the equation, a generalized EOS for high pressure-liquids is established by using the reduced state principle and introducing a characteristic parameter-configuration factorξ.Reasonably satisfactory P-V-T data for many organic compounds, including some polar components, were calculated by using the equation.

  18. High-performance liquid chromatography of oligoguanylates at high pH

    Science.gov (United States)

    Stribling, R.; Deamer, D. (Principal Investigator)

    1991-01-01

    Because of the stable self-structures formed by oligomers of guanosine, standard high-performance liquid chromatography techniques for oligonucleotide fractionation are not applicable. Previously, oligoguanylate separations have been carried out at pH 12 using RPC-5 as the packing material. While RPC-5 provides excellent separations, there are several limitations, including the lack of a commercially available source. This report describes a new anion-exchange high-performance liquid chromatography method using HEMA-IEC BIO Q, which successfully separates different forms of the guanosine monomer as well as longer oligoguanylates. The reproducibility and stability at high pH suggests a versatile role for this material.

  19. Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.

    Science.gov (United States)

    Celano, Rita; Piccinelli, Anna Lisa; Campone, Luca; Rastrelli, Luca

    2014-08-15

    Pharmaceutical and personal care products (PPCPs) are one of the most important classes of emerging contaminants. The potential of ecological and environmental impacts associated with PPCPs are of particular concern because they continually penetrate the aquatic environment. This work describes a novel ultra-preconcentration technique for the rapid and highly sensitive analysis of selected PPCPs in environmental water matrices at ppt levels. Selected PPCPs were rapidly extracted and concentrated from large volumes of aqueous solutions (500 and 250mL) by solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and then analyzed using UHPLC-MS/MS. Experimental parameters were carefully investigated and optimized to achieve the best SPE-DLLME efficiency and higher enrichment factors. The best results were obtained using the ternary mixture acetonitrile/methanol/dichloromethane 3:3:4, v/v/v, both as SPE eluent and DLLME extractant/dispersive mixture. DLLME aqueous solution (5% NaCl, 10mgL(-1) TBAB) was also modified to improve the extraction efficiency of more hydrophilic PPCPs. Under the optimal conditions, an exhaustive extraction for most of the investigated analytes (recoveries >70%), with a precision (RSD <10%) and very high enrichment factors were attained for different aqueous matrices (drinking, sea, river and wastewater). Method detection and quantification limits were at very low ppt levels and below 1 and 3ngL(-1), respectively, for 15 of selected PPCPs. The proposed analytical procedure offers numerous advantages such as the simplicity of operation, rapidity, a high enrichment factor and sensitivity. So it is suitable for monitoring and studies of occurrence of PPCPs in different environmental compartments.

  20. Determination of saffron quality by high-performance liquid chromatography.

    Science.gov (United States)

    Valle García-Rodríguez, M; Serrano-Díaz, Jéssica; Tarantilis, Petros A; López-Córcoles, Horacio; Carmona, Manuel; Alonso, Gonzalo L

    2014-08-13

    The aim of this work was to propose a high-performance liquid chromatography with diode array detection (HPLC-DAD) method for determining the three main compounds responsible for determining the quality of saffron (crocetin esters, picrocrocin, and safranal) by preparing an aqueous extract according to the ISO 3632 standard to solve the difficulty that this standard has for aroma and taste determination by ultraviolet-visible spectroscopy. Toward this aim, laboratory-isolated picrocrocin, a safranal standard with a purity of ≥ 88%, trans-crocetin di(β-D-gentiobiosyl) ester (trans-4-GG) and trans-crocetin (β-D-glucosyl)-(β-D-gentiobiosyl) ester (trans-3-Gg) standards, both with a purity of ≥ 99%, and 50 different saffron spice samples from Italy, Iran, Greece, and Spain were used in the intralaboratory validation of the HPLC method. The analytical method proposed was adequate in terms of linearity, selectivity, sensitivity, and accuracy for determining the three foremost parameters that define the quality of saffron using only a saffron solution prepared according to the ISO 3632 standard.

  1. Sheath liquid effects in capillary high-performance liquid chromatography-electrospray mass spectrometry of oligonucleotides.

    Science.gov (United States)

    Huber, C G; Krajete, A

    2000-02-18

    Fused-silica capillary columns of 200 microm inner diameter were packed with micropellicular, octadecylated, 2.3 microm poly(styrene-divinylbenzene) particles and applied to the separation of oligonucleotides by ion-pair reversed-phase high-performance liquid chromatography. Oligonucleotides were eluted at 50 degrees C with gradients of 3-13% acetonitrile in 50 mM triethylammonium bicarbonate. Addition of sheath liquid to the column effluent allowed the detection of oligonucleotides by electrospray ionization mass spectrometry using full-scan data acquisition with a detectability comparable to that obtained with UV detection. The signal-to-noise ratios with different sheath liquids increased in the order isopropanolliquid was found to influence the charge state distribution of oligonucleotides longer than 20 nucleotide units whereas no significant effect was observed with shorter oligonucleotides. Organic acids and bases in the sheath liquid generally deteriorated the signal-to-noise ratios in the chromatograms and mass spectra mainly because of increased background noise. Only a few charge states were observed in the mass spectra of oligonucleotides because of charge state reduction due to the presence of carbonic acid in the eluent. With triethylammonium hydrogencarbonate as chromatographic eluent and acetonitrile as sheath liquid, very few cation adducts of oligonucleotides were observed in the mass spectra. However, the presence of small amounts of monopotassium adducts enabled the calculation of the charge state of multiply charged ions. With acetonitrile as sheath liquid, 710 amol of a 16-mer oligonucleotide were detected using selected ion monitoring data acquisition with a signal-to-noise ratio of 3:1. Finally, capillary ion-pair reversed-phase high-performance liquid chromatography-electrospray ionization mass spectrometry was

  2. Distribution of C16:0, C18:0, C24:1, and C24:0 sulfatides in central nervous system lipid rafts by quantitative ultra-high-pressure liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Moyano, Ana Lis; Li, Guannan; Lopez-Rosas, Aurora; Månsson, Jan-Eric; van Breemen, Richard B; Givogri, Maria Irene

    2014-12-15

    Sulfated galactosylceramides (sulfatides) are glycosphingolipids associated with cholesterol- and sphingolipid-enriched membrane microdomains (lipid rafts) and are highly expressed in brain tissue. Although it is known that sulfatide species show heterogeneity in their fatty acid acyl group composition throughout brain development, their lipid raft distribution and biological relevance is poorly understood. We validated a fast and sensitive ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method to measure developmentally regulated sulfatide species (C16:0, C18:0, C24:1, and C24:0) in central nervous system (CNS) lipid rafts isolated without using detergent. Our UHPLC-MS/MS assay showed good accuracy and precision with a linear range of 5 to 1,000 nM for C18:0 and C24:1 sulfatides and 10 to 1,000 nM for C16:0 and C24:0 sulfatides. We applied this quantitative analysis to detergent-free lipid rafts isolated from wild-type mice and arylsulfatase A-deficient (ASA knockout) mice that accumulate sulfatides. All four sulfatide species were more abundant in raft membranes than in non-raft membranes, with a significant increase in lipid rafts isolated from ASA knockout mice. This is the first description of an analytical method to study these sulfatide species in raft and non-raft membranes and has the potential to be applied to preparations from other tissues.

  3. Determination of tocopherols and tocotrienols in cereals by pressurized liquid extraction-liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Bustamante-Rangel, M; Delgado-Zamarreño, M M; Sánchez-Pérez, A; Carabias-Martínez, R

    2007-03-28

    A rapid analytical method including pressurized liquid extraction (PLE) and liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) has been developed for the determination of tocopherols and tocotrienols in cereals. The pressurized liquid extraction parameters were optimized in order to maximize the extraction efficiency. The use of methanol as extraction solvent at a temperature of 50 degrees C and a pressure of 110 bar, using one cycle of extraction with a static time of 5 min, provided the best results. A good LC separation was achieved using a C(18) column and a solution of 6.0 mM ammonia in methanol/water (97:3, v/v) as the mobile phase at a flow rate of 0.2 mL min(-1). MS coupling with an ESI interface in the negative ion mode was used as the detection technique. In the present work, it is shown that the addition of a base to the mobile phase is required to enhance the ionization of tocopherols and tocotrienols in negative ion mode electrospray ionization. The applicability of the method to cereal samples was confirmed. The reproducibility of the procedure was good, with relative standard deviations in the 6-10% range. The recoveries of added tocopherols from cereal samples ranged from 91 to 109%.

  4. A Method for the Quantitation of Trace Levels of Dimethyl Sulfoxide in Urine by High Performance Liquid Chromatography

    Science.gov (United States)

    1989-05-01

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY by...for the sample cleanup and concentration, followed by separation by reversed phase high performance liquid chromatography . EXPERIMENTAL Materials...DIMETHYL SULFOXIDE IN URINE BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY 4. AUTHORS (Last name, first name, middle initial. If military, show rank, e.g.

  5. Determination of Dimethyl Sulfoxide (DMSO), Ethanol (ETOH), Formamide (F) and Glycerol/Formal (GF) by High Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    1989-01-30

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC...Classification) (U) Determination of Dimethyl Sulfoxide (DMSO), Ethanol, (ETOH), Formamide (F), and Glycerol/ Formal (GF) by High Performance Liquid Chromatography (HPLC...and 5). High performance liquid chromatography (HPLC) was the analytical method of choice for analyzing DMSO, ethanol, formamide and

  6. Determination of 5-Bromo-2’-Deoxyuridine (BrdU) in Well Water by High Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    1992-09-01

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC...Securrty Classification) Determination of 5-Bromo-2’-Deoxyuridine (BrdU) in Well Water by High Performance Liquid Chromatography (hPLC) 12. PERSONAL...PLOT OF BrdU STABILITY VERSUS TIME ....................... 10 ii DETERMINATION OF 5-BROMO-2’-DEOXY-URIDINE (BrdU) IN WELL WATER BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

  7. A comparative study on analytical method of total alkaloids from cortex Phellodendri amurens by reversed phase high performance liquid chromatography (RP-HPLC and pressurized capillary electrochromatography (pCEC

    Directory of Open Access Journals (Sweden)

    Bo Yang

    2011-02-01

    Full Text Available A pressurized capillary electrochromatography (pCEC method with post-column detection cell has been developed for the analysis of total alkaloids of cortex Phellodendron amurense Rupr., Rutaceae. The separation of total alkaloids (berberine, palmatine, oatrorrhizine, magnoflorine, phellodendrine, candicine, menisperine was optimized by compositions of the mobile phase, ionic strength of buffers, pH value, and applied voltage. Separation of total alkaloids was achieved within 11 min by using a mobile phase of Na2HPO4-citric acid solution-acetonitrile (pH 4.00; 3 mM (60:40, v/v and applying a voltage of -10 kV. This method showed satisfactory retention times and peak shapes. Meanwhile, a reversed phase high performance liquid chromatography (RP-HPLC has also been established for the separation of total alkaloids extracted from cortex Phellodendri amurens. Baseline separation of total alkaloids was achieved within 25 min by using a mobile phase of acetonitrile-0.1% phosphoric acid with 0.1 g sodium dodecanesulphonate per 100 mL (35:65, v/v. Compared to conventional RP-HPLC, pCEC led to higher column efficiency, less consumption of reagent, and shorter analysis time.

  8. Fast, rugged and sensitive ultra high pressure liquid chromatography tandem mass spectrometry method for analysis of cyanotoxins in raw water and drinking water--First findings of anatoxins, cylindrospermopsins and microcystin variants in Swedish source waters and infiltration ponds.

    Science.gov (United States)

    Pekar, Heidi; Westerberg, Erik; Bruno, Oscar; Lääne, Ants; Persson, Kenneth M; Sundström, L Fredrik; Thim, Anna-Maria

    2016-01-15

    Freshwater blooms of cyanobacteria (blue-green algae) in source waters are generally composed of several different strains with the capability to produce a variety of toxins. The major exposure routes for humans are direct contact with recreational waters and ingestion of drinking water not efficiently treated. The ultra high pressure liquid chromatography tandem mass spectrometry based analytical method presented here allows simultaneous analysis of 22 cyanotoxins from different toxin groups, including anatoxins, cylindrospermopsins, nodularin and microcystins in raw water and drinking water. The use of reference standards enables correct identification of toxins as well as precision of the quantification and due to matrix effects, recovery correction is required. The multi-toxin group method presented here, does not compromise sensitivity, despite the large number of analytes. The limit of quantification was set to 0.1 μg/L for 75% of the cyanotoxins in drinking water and 0.5 μg/L for all cyanotoxins in raw water, which is compliant with the WHO guidance value for microcystin-LR. The matrix effects experienced during analysis were reasonable for most analytes, considering the large volume injected into the mass spectrometer. The time of analysis, including lysing of cell bound toxins, is less than three hours. Furthermore, the method was tested in Swedish source waters and infiltration ponds resulting in evidence of presence of anatoxin, homo-anatoxin, cylindrospermopsin and several variants of microcystins for the first time in Sweden, proving its usefulness.

  9. Comparison of microbial communities in Lake Tahoe surface sample with Tonga Trench water column samples using High Pressure Liquid Chromatography - Electrospray Ionization - Mass Spectroscopy (HPLC - ESI - MS) and Global Natural Products Social Molecular Network (GNPS)

    Science.gov (United States)

    Belmonte, M. A.

    2015-12-01

    Intact polar lipids (IPLs) are lipids composed of a head group, a glycerol, and a fatty acid chain that make up the lipid bilayer of cell membranes in living cells; and the varying head groups can be indicative of the type of microbes present in the environment (Van Mooy 2010). So by distinguishing and identifying the IPL distribution in an environment one can make inferences about the microbial communities in the said environment. In this study, we used High Pressure Liquid Chromatography-Electrospray Ionization- Mass Spectroscopy (HPLC-ESI-MS) and Global Natural Products Social Molecular Networking (GNPS) to compare the IPL distributions of two oligotrophic environments: surface waters of Lake Tahoe in the Sierra Nevada Mountains, and the water column of the Tonga Trench in the South Pacific. We hypothesized that the similar nutrient dynamics of the two oligotrophic environments would result in similar eukaryotic and prokaryotic communities, which would be reflected in the IPL composition of suspended particulate organic matter (POM). For simplicity we focused on the classes of IPLs most commonly observed in the marine environment: phosphotidylglycerol (PG), phosphotidylethanolamine (PE), diacylglyceryl-trimethyl-homoserine (DGTS), diacylglyceryl-hydroxymethyl-trimethylalanine (DGTA), sulfoquinovosyldiacylglycerol (SQDG), monoglycosyldiacylglycerol (MGDG) and diglycosyldiacylglycerol (DGDG). Our results showed that all of the marine IPLs of interest were present in Lake Tahoe which confirms that there are many of the same microbial communities in the fresh waters of Lake Tahoe and the salt waters Tonga Trench.

  10. Achieving quasi-adiabatic thermal environment to maximize resolution power in very high-pressure liquid chromatography: Theory, models, and experiments.

    Science.gov (United States)

    Gritti, Fabrice; Gilar, Martin; Jarrell, Joseph A

    2016-04-29

    A cylindrical vacuum chamber (inner diameter 5 cm) housing a narrow-bore 2.1 mm×100 mm column packed with 1.8 μm HSS-T3 fully porous particles was built in order to isolate thermally the chromatographic column from the external air environment. Consistent with statistical physics and the mean free path of air molecules, the experimental results show that natural air convection and conduction are fully eliminated for housing air pressures smaller than 10(-4) Torr. Heat radiation is minimized by wrapping up the column with low-emissivity aluminum-tape (emissivity coefficient ϵ=0.03 vs. 0.28 for polished stainless steel 316). Overall, the heat flux at the column wall is reduced by 96% with respect to standard still-air ovens. From a practical viewpoint, the efficiency of the column run at a flow rate of 0.6 mL/min at a constant 13,000 psi pressure drop (the viscous heat power is around 9 W/m) is improved by up to 35% irrespective of the analyte retention. Models of heat and mass transfer reveal that (1) the amplitude of the radial temperature gradient is significantly reduced from 0.30 to 0.01 K and (2) the observed improvement in resolution power stems from a more uniform distribution of the flow velocity across the column diameter. The eddy dispersion term in the van Deemter equation is reduced by 0.8±0.1 reduced plate height unit, a significant gain in column performance.

  11. Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-01-01

    A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

  12. Application of High Performance Liquid Chromatography to Separation of Novel Chiral Tetrahedral Heterometal Clusters

    Institute of Scientific and Technical Information of China (English)

    Xin Yi ZHU; Wei Qiang ZHANG; Yu Hua ZHANG; Li Ren CHEN; Yong Min LI

    2003-01-01

    A series of novel chiral tetrahedral heterometal clusters have firstly been separated oncellulose tris-(3,5-dimethylphenylcarbamate) stationary phase by high performance liquid chrom-atography, using hexane as the mobile phase with various alcohols as modifiers.

  13. Differential coulometric oxidation following post column-switching high pressure liquid chromatography for fluorescence measurement of unmetabolized folic acid in human plasma.

    Science.gov (United States)

    Bailey, Steven W; Ayling, June E

    2013-11-08

    Although many countries have fortified their grain supplies with folic acid (FA) to decrease the incidence of neural tube defects, others have not due to concerns that this synthetic folate might have some adverse effects. Persistent unmetabolized FA has been found even in plasma from fasted subjects. To facilitate measurement of low levels of folic acid in human plasma, post-column coulometric oxidative cleavage was used to convert poorly fluorescent FA into a highly fluorescent compound determined to be 6-formyl-pterin. To minimize sample work-up and maximize recovery, column-switching HPLC transferred a window of eluate containing the FA from the first column (C8) onto a second column (phenyl-hexyl). The pH of two mobile phases were adjusted to be above and then below a pK of the FA α-carboxyl group, thus promoting separation from compounds coeluting from the C8-column. This permitted sample preparation using only a simple high recovery protein precipitation. Definitive identification of FA in human plasma was accomplished by duplicate injections of sample with the electrochemical voltage set above and below its half-potential. The LOD (S/N=3) was 0.10 nM. The intra- and inter-assay CV's were 2.3% and 5%, respectively. Comparison of these results with those obtained by HPLC/MS/MS with stable isotope internal standard showed a slope of 1.00 ± 0.019. This simple, sensitive, and repeatable assay facilitates a more thorough investigation of the response of various human populations to folic acid intake. Post-column differential coulometric electrochemistry can expand the variety of compounds amenable to fluorescence detection.

  14. Determination of kava lactones in food supplements by liquid chromatography-atmospheric pressure chemical ionisation tandem mass spectrometry

    NARCIS (Netherlands)

    Bobeldijk, I.; Boonzaaijer, G.; Spies-Faber, E.J.; Vaes, W.H.J.

    2005-01-01

    Reversed-phase liquid chromatography and detection with atmospheric pressure chemical ionisation tandem mass spectrometry was used for the determination of kava extracts in herbal mixtures. One percent of kava extract can be detected, corresponding to approximately 0.05-0.2 mg/g of the individual ka

  15. Ultrasonic level sensors for liquids under high pressure

    Science.gov (United States)

    Zuckerwar, A. J.; Mazel, D. S.; Hodges, D. Y.

    1986-01-01

    An ultrasonic level sensor of novel design continuously measures the level of a liquid subjected to a high pressure (up to about 40 MPa), as is sometimes required for the effective transfer of the liquid. The sensor operates as a composite resonator fabricated from a standard high-pressure plug. A flat-bottom hole is machined into the plug along its center line. An ultrasonic transducer is bonded rigidly to the interior surface of the bottom wall, while the exterior surface is in contact with the liquid. Although the bottom wall is designed to satisfy the pressure code, it is still sufficiently thin to permit ready excitation of the axisymmetric plate modes of vibration. The liquid level is measured by a conventional pulse-echo technique. A prototype sensor was tested successfully in a 2300-l water vessel at pressures up to about 37 MPa. A spectral analysis of the transmitted pulse reveals that the flexural, extensional, thickness-shear, and radial plate modes are excited into vibration, but none of these appears to be significantly affected by the pressurization of the liquid.

  16. Identification of photodegradation product of amisulpride by ultra-high-pressure liquid chromatography-DAD/ESI-quadrupole time-of-flight-mass spectrometry.

    Science.gov (United States)

    Skibiński, Robert

    2011-12-15

    Photostability of amisulpride under UVA irradiation in methanol solution was investigated and structural elucidation of its photodegradation products was performed. For the purpose of the quantitative and qualitative analysis of amisulpride and the stress degradation products elucidation, the reversed phase UHPLC-DAD system coupled with accurate mass hybrid ESI-Q-TOF mass spectrometer was used. During one run (10 min) with the use of auto MS/MS mode all essential data for the determination of photodegradation kinetics and for the structural formulas elucidation of the products was collected. Four degradation products were found and their masses with high accuracy (0.53-3.05 ppm) and formulas were obtained--258.0666 (C(10)H(14)N(2)O(4)S), 367.1564 (C(17)H(25)N(3)O(4)S), 341.1412 (C(15)H(23)N(3)O(4)S) and 385.1665 (C(17)H(27)N(3)O(5)S). For all the analyzed compounds MS/MS fragmentation spectra were obtained (collision energy 19.8-26.1 V) allowing structural elucidation of unknown degradation products and indicating photodegradation pathways of amisulpride. UHPLC-DAD/ESI-Q-TOF system was found to be a powerful analytical tool for the fast and accurate stability analysis of pharmaceutical substances.

  17. New methods and materials for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Dumont, Philip John [Iowa State Univ., Ames, IA (United States)

    1996-04-23

    This paper describes methods for solid phase extraction and high performance liquid chromatography (HPLC). The following are described: Effects of Resin Sulfonation on the Retention of Polar Organic Compounds in Solid Phase Extraction; Ion-Chromatographic Separation of Alkali Metals In Non-Aqueous Solvents; Cation-Exchange Chromatography in Non-Aqueous Solvents; and Silicalite As a Stationary Phase For HPLC.

  18. Detection of vitamin B6 in beverage by high pressure liquid chromatography%高压液相色谱法检测饮料中维生素B6

    Institute of Scientific and Technical Information of China (English)

    何珊丽; 胡燕玲; 梁波

    2013-01-01

      目的建立饮料中维生素 B6含量的高压液相色谱检测方法。方法饮料样品经稀释、过滤后,用高压液相色谱仪进行测定,测定结果与 GB/T 5009.154-2003《食品中维生素 B6的测定》比较。结果浓度范围内线性关系良好,相关系数r均在0.999以上。本方法的检出限(S/N≥3)为吡哆醇15μg/kg、吡哆醛13μg/kg、吡哆胺16μg/kg。平均回收率为98.9%~99.5%,相对标准偏差为0.88%~1.05%。使用高压液相色谱法测定饮料中维生素 B6的含量与使用微生物方法检测得到的数据一致,而高压液相色谱法所用时间比微生物法要短得多。结论高压液相色谱法测定饮料中维生素B6灵敏度高,值得在实验室的日常检测中推广。%  Objective To establish a rapid and effective method for the detection of vitamin B6 in beve-rage by high pressure liquid chromatography (HPLC). Methods After dilution and filtration, samples was measured by high pressure liquid chromatography with fluorescence detector, and the data was compared with that obtained by the national standard microbial method. Results The method showed a good linearity with r≥0.999. The LODs of pyridoxine, pyridoxal and pyridoxmine were 15, 13, 16μg/kg, respectively. The recoveries were 98.9%~99.5%and the relative standard deviations were 0.88%~1.05%.The data of vitamin B6 content in beverage detected by HPLC was consistent with that obtained by microbial method. But the detection time of HPLC was much shorter than that of the microbial method. Moreover, the operation of HPLC was simple, and the repeata-bility and accuracy of data were much higher as well. Conclusion HPLC is a sensitive method for the detec-tion of vitamin B6 in beverage, and it could be applied to the daily detection in laboratory.

  19. An improved high performance liquid chromatography-photodiode array detection-atmospheric pressure chemical ionization-mass spectrometry method for determination of chlorophylls and their derivatives in freeze-dried and hot-air-dried Rhinacanthus nasutus (L.) Kurz.

    Science.gov (United States)

    Kao, Tsai Hua; Chen, Chia Ju; Chen, Bing Huei

    2011-10-30

    Rhinacanthus nasutus (L.) Kurz, a traditional Chinese herb possessing antioxidant and anti-cancer activities, has been reported to contain functional components like carotenoids and chlorophylls. However, the variety and amount of chlorophylls remain uncertain. The objectives of this study were to develop a high performance liquid chromatography-photodiode array detection-atmospheric pressure chemical ionization-mass spectrometry (HPLC-DAD-APCI-MS) method for determination of chlorophylls and their derivatives in hot-air-dried and freeze-dried R. nasutus. An Agilent Eclipse XDB-C18 column and a gradient mobile phase composed of methanol/N,N-dimethylformamide (97:3, v/v), acetonitrile and acetone were employed to separate internal standard zinc-phthalocyanine plus 12 cholorophylls and their derivatives within 21 min, including chlorophyll a, chlorophyll a', hydroxychlorophyll a, 15-OH-lactone chlorophyll a, chlorophyll b, chlorophyll b', hydroxychlorophyll b, pheophytin a, pheophytin a', hydroxypheophytin a, hydroxypheophytin a' and pheophytin b in hot-air-dried R. nasutus with flow rate at 1 mL/min and detection at 660 nm. But, in freeze-dried R. nasutus, only 4 chlorophylls and their derivatives, including chlorophyll a, chlorophyll a', chlorophyll b and pheophytin a were detected. Zinc-phthalocyanine was found to be an appropriate internal standard to quantify all the chlorophyll compounds. After quantification by HPLC-DAD, both chlorophyll a and pheophytin a were the most abundant in hot-air-dried R. nasutus, while in freeze-dried R. nasutus, chlorophyll a and chlorophyll b dominated.

  20. Cobalamin Concentrations in Fetal Liver Show Gender Differences: A Result from Using a High-Pressure Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry as an Ultratrace Cobalt Speciation Method.

    Science.gov (United States)

    Bosle, Janine; Goetz, Sven; Raab, Andrea; Krupp, Eva M; Scheckel, Kirk G; Lombi, Enzo; Meharg, Andrew A; Fowler, Paul A; Feldmann, Jörg

    2016-12-20

    Maternal diet and lifestyle choices may affect placental transfer of cobalamin (Cbl) to the fetus. Fetal liver concentration of Cbl reflects nutritional status with regards to vitamin B12, but at these low concentration current Cbl measurement methods lack robustness. An analytical method based on enzymatic extraction with subsequent reversed-phase-high-pressure liquid chromatography (RP-HPLC) separation and parallel ICPMS and electrospray ionization (ESI)-Orbitrap-MS to determine specifically Cbl species in liver samples of only 10-50 mg was developed using 14 pig livers. Subsequently 55 human fetal livers were analyzed. HPLC-ICPMS analysis for cobalt (Co) and Cbl gave detection limits of 0.18 ng/g and 0.88 ng/g d.m. in liver samples, respectively, with a recovery of >95%. Total Co (Cot) concentration did not reflect the amount of Cbl or vitamin B12 in the liver. Cbl bound Co contributes only 45 ± 15% to Cot. XRF mapping and μXANES analysis confirmed the occurrence of non-Cbl cobalt in pig liver hot spots indicating particular Co. No correlations of total cobalt nor Cbl with fetal weight or weeks of gestation were found for the human fetal livers. Although no gender difference could be identified for total Co concentration, female livers were significantly higher in Cbl concentration (24.1 ± 7.8 ng/g) than those from male fetuses (19.8 ± 7.1 ng/g) (p = 0.04). This HPLC-ICPMS method was able to quantify total Cot and Cbl in fetus liver, and it was sensitive and precise enough to identify this gender difference.

  1. Ion suppression and enhancement effects of co-eluting analytes in multi-analyte approaches: systematic investigation using ultra-high-performance liquid chromatography/mass spectrometry with atmospheric-pressure chemical ionization or electrospray ionization.

    Science.gov (United States)

    Remane, Daniela; Meyer, Markus R; Wissenbach, Dirk K; Maurer, Hans H

    2010-11-15

    In multi-analyte procedures, sufficient separation is important to avoid interferences, particularly when using liquid chromatography/mass spectrometry (LC/MS) because of possible ion suppression or enhancement. However, even using ultra-high-performance LC, baseline separation is not always possible. For development and validation of an LC/MS/MS approach for quantification of 140 antidepressants, benzodiazepines, neuroleptics, beta-blockers, oral antidiabetics, and analytes measured in the context of brain death diagnosis in plasma, the extent of ion suppression or enhancement of co-eluting analytes within and between the drug classes was investigated using atmospheric-pressure chemical ionization (APCI) or electrospray ionization (ESI). Within the drug classes, five analytes showed ion enhancement of over 25% and six analytes ion suppression of over 25% using APCI and 16 analytes ion suppression of over 25% using ESI. Between the drug classes, two analytes showed ion suppression of over 25% using APCI. Using ESI, one analyte showed ion enhancement of over 25% and five analytes ion suppression of over 25%. These effects may influence the drug quantification using calibrators made in presence of overlapping and thus interfering analytes. Ion suppression/enhancement effects induced by co-eluting drugs of different classes present in the patient sample may also lead to false measurements using class-specific calibrators made in absence of overlapping and thus interfering analytes. In conclusion, ion suppression and enhancement tests are essential during method development and validation in LC/MS/MS multi-analyte procedures, with special regards to co-eluting analytes.

  2. Determination of 17a-Mehthyltestosterone Residue in T. niloticus Using High Pressure Liquid Chromatography%罗非鱼中甲基睾酮超高压液相色谱测定方法

    Institute of Scientific and Technical Information of China (English)

    秦安丽

    2011-01-01

    超高压液相色谱法测定罗非鱼中的甲基睾酮残留。样品经乙醚超声波提取、石油醚纯化,以BEHC18柱、70%甲醇溶液洗脱分离,PDA检测器,外标法定量。结果表明,回收率不低于80%,相对标准偏差不高于6.50%,定量限为8mg/kg。该法准确可行、前处理简便、适用于批量样品的检测。%High pressure liquid chromatography of 17a-Mehthyltestosterone residue in T.niloticus. Sam- ples were extracted using ether with the assistance of ultrasonic and cleaned up using petroleum ether. The chromatographic separation was achieved on BEH-C18coumn using 70% aqueous methanol solution as an eluant. 17a-MeT was detected using a uv detector and quantified by external standard method. The method revealed spike recoveries for 17a-Mehthyltestosterone in the muscles of T. niloticus of not less than 80% With relative standard deviations of not more than 6% and a limit of quantification of 8 ug/kg. The method, thanks to its simplicity and accuracy, is most suitable for the determination of 17a-MeT1 residue in large quantities of samples.

  3. Simultaneous determination of cyclodol and diprazin by thin layer chromatography and high performance liquid chromatography.

    Science.gov (United States)

    Makharadze, R; Adeishvili, L; Chelidze, T; Imnadze, N; Nizharadze, N

    2009-11-01

    Ciklodol (trihexyphenidil)--the central and peripheral m-cholinoblocker is currently used with other antipsychotic drugs such as phenotiazines and tricycle antidepressants. For the purpose of simultaneous determination of ciklodol and diprazine, were selected two methods of analysis: Thin Layer Chromatography (TLC) and High Performance Liquid Chromatography (HPLC). During development of TLC method was studied the 10 visualizing system and 24 mobile systems. For individual or simultaneous determination of ciklodol and diprazine were recommended the following solvents' systems: 1. Toluene-acetone-ethanole-25%NH(4)OH (45:45: 7.5:2.5), 2. Hexane-ethyl acetate (15:5), 3. Chloroform-heptene-25%NH(4)OH (16:3:3), 4. Ethylacetate-hexane (10:10), 5. Acetonitrile-metanol (10:10) and 6.Heptene-chloroform-ethanol-25% NH(4)OH (5:10:3:1). As visualizing systems were chosen: Iodine vapors, blacklight (UV254) and reagent of FNP. Reagent of FNP gives colored spot just with diprazine and it is also could be used for separation of both objects in simultaneous analysis. Developed HPLC method of simultaneous determination of ciklodol and diprazine: like mobile phase is recommended: Acetonitril- 0.05M KH(2)PO4 (55:45) (v/v) +H(3)PO(4) (pH3.5), column EC250 x 4.6mm, with solid phase Nucleosil, flow rate 1ml/min, sample volume 40 microl. In given conditions, the retention time of ciklodol is 6.005min and diprazine 7.227min. Developed method of simultaneous determination and separation of ciklodol and diprazine in respective mixtures could be successfully applied as in the pharmaceutical, as well in the chemical-toxicological laboratories.

  4. Resolution of RNA using high-performance liquid chromatography

    NARCIS (Netherlands)

    Mclaughlin, L.W.; Bischoff, Rainer

    1987-01-01

    High-performance liquid chromatographic techniques can be very effective for the resolution and isolation of nucleic acids. The characteristic ionic (phosphodiesters) and hydrophobic (nucleobases) properties of RNAs can be exploited for their separation. In this respect anion-exchange and reversed-p

  5. Equation of state of liquid Indium under high pressure

    Directory of Open Access Journals (Sweden)

    Huaming Li

    2015-09-01

    Full Text Available We apply an equation of state of a power law form to liquid Indium to study its thermodynamic properties under high temperature and high pressure. Molar volume of molten indium is calculated along the isothermal line at 710K within good precision as compared with the experimental data in an externally heated diamond anvil cell. Bulk modulus, thermal expansion and internal pressure are obtained for isothermal compression. Other thermodynamic properties are also calculated along the fitted high pressure melting line. While our results suggest that the power law form may be a better choice for the equation of state of liquids, these detailed predictions are yet to be confirmed by further experiment.

  6. High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids

    DEFF Research Database (Denmark)

    Lue, Bena-Marie; Guo, Zheng; Xu, X.B.

    2008-01-01

    Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found...

  7. Analysis of carotenoid and porphyrin pigments of geochemical interest by high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Hajibrahim, S.K. (Univ. of Bristol, Eng.); Tibbetts, P.J.C.; Watts, C.D.; Maxwell, J.R.; Eglinton, G.; Colin, H.; Guiochon, G.

    1978-04-01

    High-performance liquid chromatography (HPLC) is shown to be a powerful tool in the analysis of carotenoid and porphyrin pigments. Columns packed with 5-..mu..m irregular silica gel particles by a high density and high constant pressure method allow efficient separation of mixtures of total nonsaponifiable carotenoids from recent sedimentary situations. Good reproducibility of retention times (within 2%) is achieved in the gradient elution mode. However, attention must be paid to reequilibration of the column after each injection by washing with the less polar solvent for a minimum of 15 min (for carotenoids) or of 30 min (for porphyrins). HPLC appears to be useful in ''fingerprinting'' petroporphyrin distributions in crude oil.

  8. Differentiation of coloured inks of inkjet printer cartridges by thin layer chromatography and high performance liquid chromatography.

    Science.gov (United States)

    Poon, N L; Ho, S S H; Li, C K

    2005-01-01

    Document examiners are frequently asked to determine whether or not a colour printout has originated from a particular inkjet printer. The printer can rarely be identified unless some unique defects or irregularities of the printer are present on the printout. However, it is possible to decipher the make and/or model of the printer by comparing the ink-profile of the questioned printout with that of a seized inkjet printer cartridge or from one in a database. This paper presents an overview of a systematic approach to characterising and discriminating the inks of different inkjet printer cartridges using thin layer chromatography (TLC) and high pressure liquid chromatography (HPLC) with multi-wavelength ultra-violet/visible (UV/Vis) detection. Ink samples from 23 different inkjet printer cartridges (including originals and substitutes) of different brands and colour printouts, printed by known printers were examined with newly developed chromatographic methods. Subsequently, a database of the ink-profiles was generated. The methods provide a useful tool for discriminating coloured inks in inkjet printer cartridges of different brands.

  9. HIGH PERFORMANCE LIQUID CHROMATOGRAPHY DETECTORS – A REVIEW

    Directory of Open Access Journals (Sweden)

    Kaushal Ramni

    2011-05-01

    Full Text Available HPLC is the most versatile and widely used elution chromatography. The technique is used to resolve and determine species in a variety of organic, inorganic, biological, ionic and polymeric materials. Detector is the heart of an instrument and efficiency of system is dependent upon detecting techniques. Many types of HPLC detectors exist, each of which has some valuable performance feature such as refractive index detector, ultraviolet detector, fluorescent detector, electrochemical detector, electric conductivity detector, liquid light scattering detector, evaporative light scattering detector. Due to strong requirement for improvements in sensitivity, selectivity and other performance characteristics of the detector recent developments in conventional techniques and some other new technologies have been adopted such as laser light scattering detector, charged aerosol detector, nano quantity aerosol detector, chiral detector and pulsed amperometric detector. These detectors provide accurate concentration analysis, excellent sensitivity, wide dynamic range, consistent response and broad applicability of the drug components. Working of these detectors involve different principles such as optical techniques, aerosol based techniques, refractive methods, light scattering principle, amperometric and fluorescence. The present review enlightens both conventional and advanced techniques and compares their capabilities of analyzing drug components and need for new techniques for better and wide range of applicability.

  10. Effect of pressure on secondary structure of proteins under ultra high pressure liquid chromatographic conditions.

    Science.gov (United States)

    Makarov, Alexey; LoBrutto, Rosario; Karpinski, Paul

    2013-11-29

    There are several spectroscopic techniques such as IR and CD, that allow for analyzing protein secondary structure in solution. However, a majority of these techniques require using purified protein, concentrated enough in the solution, to produce a relevant spectrum. Fundamental principles for the usage of reversed-phase ultra high pressure liquid chromatography (UHPLC) as an alternative technique to study protein secondary structures in solution were investigated. Several "model" proteins, as well as several small ionizable and neutral molecules, were used for these studies. The studies were conducted with UHPLC in isocratic mode, using premixed mobile phases at constant flow rate and temperature. The pressure was modified by a backpressure regulator from about 6000psi to about 12,000psi. It was found that when using a mobile phase composition at which proteins were fully denatured (loss of alpha-helix secondary structure), the retention factors of the proteins increased upon pressure increase in the same manner as non-proteins. When using a mobile phase composition in which proteins were not fully denatured, it was observed that the retention factors of the proteins displayed a much steeper (by one order of magnitude) increase in retention upon pressure increase. It was concluded that in a mobile phase in which the protein is not initially fully denatured, the increase of pressure may facilitate the folding back of the protein to its native state (alpha-helix secondary structure). The impact of different mobile phase compositions on the denaturation of the proteins was studied using CD (Circular Dichroism). Moreover, the effect of flow rate on retention of proteins and small molecules was studied at constant pressure on the different pore size silicas and the impact of internal frictional heating was evaluated.

  11. The Application of High Performance Liquid Chromatography in the Analysis of Trace Rare Earth

    Institute of Scientific and Technical Information of China (English)

    WANG; Xiu-feng; DING; You-qian

    2012-01-01

    <正>Rare earth elements are very important in the field of radioanalytical chemistry, for it must be separated and determined in the measurements of burn-up and fission yield. High performance liquid chromatography has become a main method in the separation of rare earth elements due to its obvious advantages, this is, high speed of analysis, high efficiency and easy automation. The ion exchange chromatography is the main means to separate rare earth elements, especially the cation exchange

  12. The isolation of soyasaponins by fractional precipitation, solid phase extraction, and low pressure liquid chromatography.

    Science.gov (United States)

    Gurfinkel, D M; Reynolds, W F; Rao, A V

    2005-11-01

    Bioactive soyasaponins are present in soybean (Glycine max). In this study, the isolation of soyasaponins in relatively pure form (>80%) using precipitation, solid phase extraction and reverse phase low pressure liquid chromatography (RP-LPLC) is described. Soy flour soyasaponins were separated from non-saponins by methanol extraction and precipitation with ammonium sulphate. Acetylated group A soyasaponins were isolated first by solid phase extraction followed by RP-LPLC (solvent: ethanol-water). Soyasaponins, from a commercial preparation, were saponified and fractionated into deacetylated group A and group B soyasaponins by solid phase extraction (methanol-water). Partial hydrolysis of group B soyasaponins produced a mixture of soyasaponin III and soyasapogenol B monoglucuronide. RP-LPLC of deacetylated group A soyasaponins separated soyasaponin A1 and A2 (38% methanol); of group B soyasaponins isolated soyasaponin I (50% ethanol); and of the partial hydrolysate separated soyasaponin III from soyasapogenol B monoglucuronide (50% ethanol). This methodology provides soyasaponin fractions that are suitable for biological evaluation.

  13. Quality evaluation of moluodan concentrated pill using high-performance liquid chromatography fingerprinting coupled with chemometrics.

    Science.gov (United States)

    Tao, Lingyan; Zhang, Qing; Wu, Yongjiang; Liu, Xuesong

    2016-12-01

    In this study, a fast and effective high-performance liquid chromatography method was developed to obtain a fingerprint chromatogram and quantitative analysis simultaneously of four indexes including gallic acid, chlorogenic acid, albiflorin and paeoniflorin of the traditional Chinese medicine Moluodan Concentrated Pill. The method was performed by using a Waters X-bridge C18 reversed phase column on an Agilent 1200S high-performance liquid chromatography system coupled with diode array detection. The mobile phase of the high-performance liquid chromatography method was composed of 20 mmol/L phosphate solution and acetonitrile with a 1 mL/min eluent velocity, under a detection temperature of 30°C and a UV detection wavelength of 254 nm. After the methodology validation, 16 batches of Moluodan Concentrated Pill were analyzed by this high-performance liquid chromatography method and both qualitative and quantitative evaluation results were achieved by similarity analysis, principal component analysis and hierarchical cluster analysis. The results of these three chemometrics were in good agreement and all indicated that batch 10 and batch 16 showed significant differences with the other 14 batches. This suggested that the developed high-performance liquid chromatography method could be applied in the quality evaluation of Moluodan Concentrated Pill.

  14. Determination of dodecylbenzenesulphonates and ethoxylated alkylphenols in liquid pesticide formulations by high-performance liquid chromatography.

    Science.gov (United States)

    Schreuder, R H; Martijn, A

    1988-01-01

    A method is presented for determining mixtures of calcium dodecylbenzene-sulphonate (CaDBS) and ethoxylated alkylphenols in pesticidal emulsifiable concentrates. The pesticide formulations are adsorbed on a pre-concentration column. The active ingredients, the solvents and the emulsifiers are eluted successively by using solvents with increasing polarities. The various homologues of CaDBS and the ethoxylated alkylphenols are separated by reversed-phase high performance liquid chromatography using methanol-water containing tetramethylammonium bromide. The oligomers of the ethoxylated phenols are separated on an aminopropyl-modified column using a solvent gradient (propan-2-ol-water and hexane-tetrahydrofuran). Quantitative results are given for synthetic samples. The degree of ethoxylation of the ethoxylated alkylphenols has been determined and the CaDBS components characterized.

  15. A semi-automatic microextraction in packed sorbent, using a digitally controlled syringe, combined with ultra-high pressure liquid chromatography as a new and ultra-fast approach for the determination of prenylflavonoids in beers.

    Science.gov (United States)

    Gonçalves, João L; Alves, Vera L; Rodrigues, Fátima P; Figueira, José A; Câmara, José S

    2013-08-23

    In this work a highly selective and sensitive analytical procedure based on semi-automatic microextraction by packed sorbents (MEPS) technique, using a new digitally controlled syringe (eVol(®)) combined with ultra-high pressure liquid chromatography (UHPLC), is proposed to determine the prenylated chalcone derived from the hop (Humulus lupulus L.), xanthohumol (XN), and its isomeric flavonone isoxanthohumol (IXN) in beers. Extraction and UHPLC parameters were accurately optimized to achieve the highest recoveries and to enhance the analytical characteristics of the method. Important parameters affecting MEPS performance, namely the type of sorbent material (C2, C8, C18, SIL, and M1), elution solvent system, number of extraction cycles (extract-discard), sample volume, elution volume, and sample pH, were evaluated. The optimal experimental conditions involves the loading of 500μL of sample through a C18 sorbent in a MEPS syringe placed in the semi-automatic eVol(®) syringe followed by elution using 250μL of acetonitrile (ACN) in a 10 extractions cycle (about 5min for the entire sample preparation step). The obtained extract is directly analyzed in the UHPLC system using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and ACN (eluent B) in the gradient elution mode (10min total analysis). Under optimized conditions good results were obtained in terms of linearity within the established concentration range with correlation coefficients (R) values higher than 0.986, with a residual deviation for each calibration point below 12%. The limit of detection (LOD) and limit of quantification (LOQ) obtained were 0.4ngmL(-1) and 1.0ngmL(-1) for IXN, and 0.9ngmL(-1) and 3.0ngmL(-1) for XN, respectively. Precision was lower than 4.6% for IXN and 8.4% for XN. Typical recoveries ranged between 67.1% and 99.3% for IXN and between 74.2% and 99.9% for XN, with relative standard deviations %RSD no larger than 8%. The applicability of the proposed analytical

  16. Pressurized nano-liquid-junction interface for coupling capillary electrochromatography and nano-liquid chromatography with mass spectrometry.

    Science.gov (United States)

    D'Orazio, Giovanni; Fanali, Salvatore

    2013-11-22

    A new nano-liquid-junction interface for coupling both capillary electrochromatography (CEC) or nano-liquid chromatography (nano-LC) with mass spectrometry (MS) was studied. The interface was a small T piece of polymeric material where capillary column and tip capillary were positioned at 180° while the third exit (at 90°) was occupied by a capillary delivering a liquid-assisting spray ionization for CEC experiments or by the electrode for the high voltage spray for nano-LC. Experiments were carried out analyzing mixtures of some organophosphorus pesticides (OPPs) or anti-inflammatory and related acidic drugs with MS detection in positive or negative ion mode, respectively. Analyzed OPPs compounds were baseline resolved utilizing the novel interface in both nano-LC and CEC obtaining good sensitivity and repeatability. For CEC-MS, the limits of detection ranged between 0.03 and 6.80 μg/mL and the intra-day repeatability was RSD interface was easy to handle and good reproducibility, between 2.5 and 3.5% for the retention time and interface was installed by two different analysts. Furthermore, it could be used for both CEC and nano-LC.

  17. Gas and high-performance liquid chromatography of phenols

    Energy Technology Data Exchange (ETDEWEB)

    Tesarova, E.; Pacakova, V.

    1983-05-01

    Gas (GC) and high-performance liquid chromatographic (HPLC) methods in the analysis of phenols are reviewed. Among the great number of phenolic compounds analyzed, alkylphenols, chlorophenols, dihydroxy-and trihydroxy-benzenes and biphenols are chiefly considered. The advantages and drawbacks of the methods are discussed. Relationships between the structural characteristics of phenols, the stationary phase structure, the mobile phase composition and the retention data are treated. Typical examples of the conditions for GC and HPLC analysis are summarized in tables. 276 references

  18. Application of Ionic Liquids in High Performance Reversed-Phase Chromatography

    Directory of Open Access Journals (Sweden)

    Wentao Bi

    2009-06-01

    Full Text Available Ionic liquids, considered “green” chemicals, are widely used in many areas of analytical chemistry due to their unique properties. Recently, ionic liquids have been used as a kind of novel additive in separation and combined with silica to synthesize new stationary phase as separation media. This review will focus on the properties and mechanisms of ionic liquids and their potential applications as mobile phase modifier and surface-bonded stationary phase in reversed-phase high performance liquid chromatography (RP-HPLC. Ionic liquids demonstrate advantages and potential in chromatographic field.

  19. Separation of Nitration By-Products in Commercial-Grade Trinitro-Toluene by High Performance Liquid Chromatography.

    Science.gov (United States)

    1982-06-01

    MRL-TN-464 SEPARATION OF NITRATION BY-PRODUCTS IN COMMERCIAL-GRADE TITR-TOLUENE BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY Peter J. Sanders ABSTRACT...UNCLASSIFIED TITLE SEPARATION OF NITRATION BY-PRODUCTS IN COMMERCIAL-GRADE TRXNITRO-TOLUENE BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY AUTHOR(S...PRODUCTS IN COMMERCIAL-GRADE TRINITRO-TOLUENE BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY 16 INTRODUCTION Fbr some time, a need has existed for the

  20. Novel determination of polychlorinated naphthalenes in water by liquid chromatography-mass spectrometry with atmospheric pressure photoionization.

    Science.gov (United States)

    Moukas, Athanasios I; Thomaidis, Nikolaos S; Calokerinos, Antony C

    2016-01-01

    This study presents the development, optimization, and validation of a novel method for the determination of polychlorinated naphthalenes (PCNs) by liquid chromatography-atmospheric pressure photoionization (APPI), using toluene as dopant. The mass spectra of PCN 52, 54, 66, 67, 73, and 75 were recorded in negative ionization. The base ions corresponded to [M-Cl+O](-), where M is the analyte molecule. A strategy, which includes designs of experiments, for the development, the evaluation, and the optimization of the LC-APPI-MS/MS methods is also described. Finally, a highly sensitive method with low instrumental limits of detection (LoDs), ranging from 0.8 pg for PCN 75 to 16 pg for PCN 54 on column, was validated. A Thermo Hypersil Green PAH (100 mm × 2.1 mm, 3 μm) column was used with acetonitrile/water/methanol as mobile phase. The method was applied for the determination of the selected PCNs in surface and tap water samples. A simple liquid-liquid extraction method for the extraction of PCNs from water samples was used. Method LoQs ranged from 29 ng L(-1), for PCN 73, to 63 ng L(-1), for PCN 54, and the recoveries ranged from 97 to 99%, for all congeners. This is the first LC-APPI-MS/MS method for the determination of PCNs in water samples.

  1. Phytochemical analysis of Hibiscus caesius using high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Ain, Quratul; Naveed, Muhammad Na; Mumtaz, Abdul Samad; Farman, Muhammad; Ahmed, Iftikhar; Khalid, Nauman

    2015-09-01

    Various species in genus Hibiscus are traditionally known for their therapeutic attributes. The present study focused on the phytochemical analysis of a rather unexplored species Hibiscus caesius (H. caesius), using high-pressure liquid chromatography coupled with mass spectrometry (HPLC-MS). The analysis revealed five major compounds in the aqueous extract, viz. vanillic acid, protocatechoic acid, quercetin, quercetin glucoside and apigenin, being reported for the first time in H. caesius. Literature suggests that these compounds have important pharmacological traits such as anti-cancer, anti-inflammatory, anti-bacterial and hepatoprotective etc. however, this requires further pharmacological investigations at in vitro and in vivo scale. The above study concluded the medicinal potential of H. caesius.

  2. Liquid Chromatography in 1982.

    Science.gov (United States)

    Freeman, David H.

    1982-01-01

    Reviews trends in liquid chromatography including apparatus, factors affecting efficient separation of a mixture (peak sharpness and speed), simplified problem-solving, adsorption, bonded phase chromatography, ion selectivity, and size exclusion. The current trend is to control chemical selectivity by the liquid phase. (Author/JN)

  3. Column Liquid Chromatography.

    Science.gov (United States)

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  4. Ionic Liquids as Mobile Phase Additives for Separation of Nucleotides in High-Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    ZHANG,Wen-Zhu(张文珠); HE,Li-Jun(何丽君); LIU,Xia(刘霞); JIANG,Sheng-Xiang(蒋生祥)

    2004-01-01

    Ionic liquids are a type of salts that are liquid at low temperature (< 100 ℃). Because of their some special properties, they have been widely used as new "green solvents" for many chemical reactions and liquid-liquid extraction in the past several years. In this paper, a new method for the separation of nucleotides is developed and the essential feature of the method is that 1-alkyl-3-methylimidazolium salts are used as mobile phase additives, resulting in a baseline separation of nucleotides without need of gradient elution and need of organic solvent addition as currently used in RP-HPLC. This study shows the potential application of ionic liquids as mobile phase additives in reversed-phase liquid chromatography.

  5. Supercooled liquid vapour pressures and related thermodynamic properties of polycyclic aromatic hydrocarbons determined by gas chromatography

    NARCIS (Netherlands)

    Haftka, J.J.H.; Parsons, J.R.; Govers, H.A.J.

    2006-01-01

    A gas chromatographic method using Kovats retention indices has been applied to determine the liquid vapour pressure (P-i), enthalpy of vaporization (Delta H-i) and difference in heat capacity between gas and liquid phase (Delta C-i) for a group of polycyclic aromatic hydrocarbons (PAHs). This group

  6. Combining Laser Ablation/Liquid Phase Collection Surface Sampling and High-Performance Liquid Chromatography Electrospray Ionization Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ovchinnikova, Olga S [ORNL; Kertesz, Vilmos [ORNL; Van Berkel, Gary J [ORNL

    2011-01-01

    This paper describes the coupling of ambient pressure transmission geometry laser ablation with a liquid phase sample collection method for surface sampling and ionization with subsequent mass spectral analysis. A commercially available autosampler was adapted to produce a liquid droplet at the end of the syringe injection needle while in close proximity to the surface to collect the sample plume produced by laser ablation. The sample collection was followed by either flow injection or a high performance liquid chromatography (HPLC) separation of the extracted components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the analytical utility of this coupling, thin films of a commercial ink sample containing rhodamine 6G and of mixed isobaric rhodamine B and 6G dyes on glass microscope slides were analyzed. The flow injection and HPLC/ESI-MS analysis revealed successful laser ablation, capture and, with HPLC, the separation of the two compounds. The ablated circular area was about 70 m in diameter for these experiments. The spatial sampling resolution afforded by the laser ablation, as well as the ability to use sample processing methods like HPLC between the sample collection and ionization steps, makes this combined surface sampling/ionization technique a highly versatile analytical tool.

  7. Heat exchanges in fast, high-performance liquid chromatography. A complete thermodynamic study

    Energy Technology Data Exchange (ETDEWEB)

    Gritti, Fabrice [University of Tennessee, Knoxville (UTK); Guiochon, Georges A [ORNL

    2008-01-01

    The successive physical transformations of the mobile phase that take place in very high pressure liquid chromatography were studied based on the formalism of classical thermodynamics. The eluent is initially under atmospheric pressure (P{sup 0}) and at ambient temperature (T{sub ext}). In a first step, it is compressed to a high pressure (P{sub max} of the order of 1 kbar) in the pump heads of the chromatograph. In a second step, the pressurized eluent is transferred to the inlet of the chromatographic column, along which, in a third step, it is decompressed to atmospheric pressure. Both the compression and the decompression of the fluid were considered to take place under conditions that can be either adiabatic or nonadiabatic and either reversible or irreversible. Applications of the first and second principles of thermodynamics allow the determination of the heat and energy exchanged between the eluent and the external surroundings during each transformation. Experimental data were acquired using acetonitrile as the mobile phase. The true state equation, {rho}(P, T), of liquid acetonitrile was used in the theoretical calculations. A series of four different flow rates (0.55, 0.85, 1.15, and 1.45 mL/min, corresponding to inlet pressures of 357.2, 559.5, 765.1, and 972.9 bar, respectively), were applied to a 2.1 x 100 mm column packed with 1.7-{micro}m bridged ethane-silicon hybrid particles. Thermocouples were used to measure the eluent temperature before and after its passage through the column. These data provide estimates of the variation of the internal energy of the eluent. The heat lost through the external wall of the column during the eluent decompression was estimated by measuring the surface temperature of the column tube under steady state. Both the compression and the decompression of acetonitrile were found to be nonadiabatic and irreversible transformations. The results showed that, during the eluent decompression, the heat released by the friction

  8. Fluorimetric assay for ornithine decarboxylase by high-performance liquid chromatography.

    Science.gov (United States)

    Haraguchi, K; Kai, M; Kohashi, K; Ohkura, Y

    1980-12-05

    A highly sensitive method for the assay of ornithine decarboxylase in sample solutions prepared from rat tissue homogenate is described which employs high-performance liquid chromatography with fluorescence detection. Putrescine formed from ornithine under the optimal conditions for the enzyme reaction is treated by Cellex P column chromatography for clean-up and converted into the fluorescamine derivative in the presence of cupric ion which inhibits the reaction of interfering amines with fluorescamine. The derivative is separated by reversed-phase chromatography on LiChrosorb RP-18 with linear gradient elution. The lower limit of detection for putrescine formed enzymatically is 5 pmol.

  9. Crosslinked polymeric ionic liquids as solid-phase microextraction sorbent coatings for high performance liquid chromatography.

    Science.gov (United States)

    Yu, Honglian; Merib, Josias; Anderson, Jared L

    2016-03-18

    Neat crosslinked polymeric ionic liquid (PIL) sorbent coatings for solid-phase microextraction (SPME) compatible with high-performance liquid chromatography (HPLC) are reported for the first time. Six structurally different PILs were crosslinked to nitinol supports and applied for the determination of select pharmaceutical drugs, phenolics, and insecticides. Sampling conditions including sample solution pH, extraction time, desorption solvent, desorption time, and desorption solvent volume were optimized using design of experiment (DOE). The developed PIL sorbent coatings were stable when performing extractions under acidic pH and remained intact in various organic desorption solvents (i.e., methanol, acetonitrile, acetone). The PIL-based sorbent coating polymerized from the IL monomer 1-vinyl-3-(10-hydroxydecyl) imidazolium chloride [VC10OHIM][Cl] and IL crosslinker 1,12-di(3-vinylbenzylimidazolium) dodecane dichloride [(VBIM)2C12] 2[Cl] exhibited superior extraction performance compared to the other studied PILs. The extraction efficiency of pharmaceutical drugs and phenolics increased when the film thickness of the PIL-based sorbent coating was increased while many insecticides were largely unaffected. Satisfactory analytical performance was obtained with limits of detection (LODs) ranging from 0.2 to 2 μg L(-1) for the target analytes. The accuracy of the analytical method was examined by studying the relative recovery of analytes in real water samples, including tap water and lake water, with recoveries varying from 50.2% to 115.9% and from 48.8% to 116.6%, respectively.

  10. [Determination of amygdalin in hawthorn by high performance liquid chromatography].

    Science.gov (United States)

    Lü, Weifeng; Ding, Mingyu

    2005-09-01

    A suitable method for extraction of amygdalin from hawthorn has been established. At first, the lipophilic components were removed with petroleum ether by ultrasonic extraction. The amygdalin was then extracted by methanol in a Soxhlet's apparatus. For quantitation, a high performance liquid chromatographic method was developed by using a reversed-phase C18 column, mobile phase of methanol-water (15:85, v/v) and a detection wavelengh of 215 nm. It can be concluded that the content of amygdalin is higher in the seeds than that in the hawthorn powder without the seeds and the yield of amygdalin is higher in the hawthorn pieces than that in the hawthorn powder.

  11. Simultaneous determination of three phenylethanoid glycosides in Cistanche tubulosa by online pressurized liquid microextraction-turbulent flow chromatography-high performance liquid chromatography%在线加压溶剂微提取-湍流色谱-高效液相色谱法同时测定管花肉苁蓉中3种苯乙醇苷

    Institute of Scientific and Technical Information of China (English)

    宋青青; 刘瑶; 张玲玲; 周利; 屠鹏飞; 宋月林

    2016-01-01

    An online pressurized liquid microextraction-turbulent flow chromatography-high performance liquid chromatography ( online PLME-TFC-HPLC ) platform was configured for simultaneous determination of three phenylethanoid glycosides in Cistanche tubulosa. Micro amount powder of crude material( 0. 5 mg ) was mixed with clean diatomaceous earth and packed into a vessel which then was put into a hollow guard column. To generate high tempera-ture and high pressure,a long polyetheretherketone(PEEK)tube(1 000 mm×0. 13 mm)was linked to the end of the hollow guard column that was warmed in the column oven( 70 ℃). The water containing 0. 1%( v/v)formic acid acted as the extraction solvent and was delivered at 2. 5 mL/min. Two electronic 6-port/2-channel valves were responsible for dividing the whole program into extraction and elution phases. The analytes were purified and enriched in a Turbo-Flow cyclone column,and back-flushed onto a Capcell PAK C 18 AQ column under a gradient elution program with 0. 1%( v/v ) aqueous formic acid-acetonitrile at the elution phase. The ultraviolet wavelength was set at 340 nm to monitor phenylethanoid glycosides. The calibration curves for the three phenylethanoid glycosides revealed good linearities in the range of 1-200 mg/L(r﹥0. 999). The limits of quantification(LOQs)were 0. 50 mg/L(echinacoside),0. 25 mg/L(acteoside)and 0. 38 mg/L(isoacteoside). The spiked recoveries were in the range of 83. 13%-114. 00% with the relative standard deviations( RSDs)between 1. 89% and 13. 34%. All the results indicated that this method is facile,efficient,reliable,and advantageous at time, labor,solvent,and material savings. The method also reduces the degradation risks and is suit-able for the determination of phenylethanoid glycosides in Cistanche tubulosa.%建立了在线加压溶剂微提取-湍流色谱-高效液相色谱( online PLME-TFC-HPLC)法,并将其应用于管花肉苁蓉中松果菊苷、毛蕊花糖苷和异毛蕊花糖苷3种

  12. Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Lee, Iris; Boyce, Mary C.

    2011-01-01

    A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

  13. Rapid determination of five food additives in soft drinks by high pressure liquid chromatography%高压液相色谱法快速测定饮料中的五种食品添加剂

    Institute of Scientific and Technical Information of China (English)

    魏杰; 郭志谋; 章飞芳; 梁鑫淼

    2013-01-01

    Objective To establish a high pressure liquid chromatography method for the simultaneous determination of 3 sweeteners (acesulfame-K, saccharin sodium, aspartame) and 2 preservatives (benzoic acid, sorbic acid) in soft drinks. Methods The samples were diluted with initial mobile phase and filtrated for liq-uid chromatographic analysis. The separation was performed on a polar-modified XAqua C18 column with 50 mmol/L pH 4.5 KH2PO4 and acetonitrile as mobile phase in gradient mode. The flow rate was set at 2 mL/min and column temperature was 40℃. The separation could be achieved within 6 min. And one sample could be analyzed within 10 min with the addition of 4 min equilibration time. Results Under the optimized chroma-tographic conditions, a good linearity was obtained in the range of 0.5~50 mg/L for the 5 food additives, with correlation coefficients (r2) all above 0.9999. For samples (carbonated and fruit juice beverage matrix) spiked with 50, 100 and 150 mg/kg of the 5 food additives, the recoveries and relative standard deviations (RSD) were96.48%~105.64% and 0.21%~5.39%, respectively. The limits of detection (LOD) of the method calculated by signal to noise ratio (S/N) = 3:1 was 0.02~0.08 mg/L. Conclusion The developed analysis method was rapid and accurate, and could be used for the simultaneous determination of sweeteners and preservatives in soft drinks.%  目的建立一种高压液相色谱方法同时检测饮料制品中3种甜味剂(安赛蜜、糖精钠、阿斯巴甜)和2种防腐剂(苯甲酸、山梨酸)。方法样品采用起始流动相稀释后直接过膜分析,色谱分离在极性修饰 XAqua C18色谱柱上进行,流动相采用50 mmol/L pH 4.5 KH2PO4和乙腈,梯度模式洗脱,流速2 mL/min,柱温40℃,6 min 内即可完成一次分离分析,加上4 min 梯度平衡时间,10 min 内即可完成平衡及分离。结果5种食品添加剂在0.5~50 mg/L 内线性关系良好,相关系数 r2均大于0.9999。

  14. Determination of Finasteride in Tablets by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    K. Basavaiah

    2007-01-01

    Full Text Available A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS in bulk drug and in tablets. FNS was eluted from a ODS C18 reversed phase column at laboratory temperature (30 ± 2°C with a mobile phase consisting of methanol and water (80+20 at a flow rate of 1 mL min-1 with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1 with limits of detection (LOD and quantification (LOQ being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

  15. Method validation for 243 pesticides and environmental contaminants in meats and poultry by tandem mass spectrometry coupled to low-pressure gas chromatography and ultra high-performance liquid chromatography

    Science.gov (United States)

    An easy and reliable high-throughput analysis method was developed and validated for 192 diverse pesticides and 51 environmental contaminants (13 PCB congeners, 14 PAHs, 7 PBDE congeners, and 17 novel flame retardants) in cattle, swine, and poultry muscle. Sample preparation was based on the “quick,...

  16. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    Science.gov (United States)

    Miller, C. J.; Elias, G.; Schmitt, N. C.; Rae, C.

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify trace levels of the military explosives, RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol and filtered using no additional sample cleanup of the sample extract prior to analysis. The filtered methanol extracts were injected directly into several different column types and analyzed by high performance liquid chromatography using ultraviolet detection and/or gas chromatography using electron capture detection. This paper describes general screening methods that were used to determine the presence of explosives (RDX, TNT, and PETN) in unknown samples of denim, colored flannel, vinyl and canvas in addition to techniques that have been optimized for quantification of each explosive from the substrate extracts.

  17. High-performance liquid chromatography of rat and mouse islet polypeptides

    DEFF Research Database (Denmark)

    Linde, S; Hansen, B; Welinder, B S

    1990-01-01

    After preparative high-performance liquid chromatography of mouse islet culture medium, concentrated on disposable C18 cartridges (Sep-Pak), an unexpected insulin immunoreactive peak eluting earlier than mouse insulin I and II was detected. Molecular mass determination by mass spectrometry...

  18. Going Beyond, Going Further: An Inexpensive Experiment for the Introduction of High Performance Liquid Chromatography.

    Science.gov (United States)

    Bidlingmeyer, Brian A.; Warren, F. Vincent, Jr.

    1984-01-01

    Background information, materials needed, laboratory procedures, and typical results are provided for five high performance liquid chromatography experiments (three isocratic and two step gradient separations). Suggestions for further experimentation are also provided, including quantitative determinations and separation of charged solutes. (JN)

  19. High-Performance Liquid Chromatography in the Undergraduate Chemical Engineering Laboratory

    Science.gov (United States)

    Frey, Douglas D.; Guo, Hui; Karnik, Nikhila

    2013-01-01

    This article describes the assembly of a simple, low-cost, high-performance liquid chromatography (HPLC) system and its use in the undergraduate chemical engineering laboratory course to perform simple experiments. By interpreting the results from these experiments students are able to gain significant experience in the general method of…

  20. DETERMINATION OF CHLOROPHENOLS, NITROPHENOLS, AND METHYLPHENOLS IN GROUND-WATER SAMPLES USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Science.gov (United States)

    A high performance liquid chromatography (HPLC) method was developed to quantitatively determine phenolic compounds and their isomers in aqueous samples. The HPLC method can analyze a mixture of 15 contaminants in the same analytical run with an analysis time of 25 minutes. The...

  1. Determination of low molecular weight thiols using monobromobimane fluorescent labeling and high-performance liquid chromatography

    Science.gov (United States)

    Fahey, Robert C.; Newton, Gerald L.

    1988-01-01

    Methods are described for the preparation and high-performance liquid chromatography (HPLC) analysis of monobromobimane derivatives of low molecular weight thiols in extracts of biological samples. Typical problems encountered in the development and application of these methods are discussed. Analysis of mung bean extract is used as an example.

  2. Sugar Determination in Foods with a Radially Compressed High Performance Liquid Chromatography Column.

    Science.gov (United States)

    Ondrus, Martin G.; And Others

    1983-01-01

    Advocates use of Waters Associates Radial Compression Separation System for high performance liquid chromatography. Discusses instrumentation and reagents, outlining procedure for analyzing various foods and discussing typical student data. Points out potential problems due to impurities and pump seal life. Suggests use of ribose as internal…

  3. An Advanced, Interactive, High-Performance Liquid Chromatography Simulator and Instructor Resources

    Science.gov (United States)

    Boswell, Paul G.; Stoll, Dwight R.; Carr, Peter W.; Nagel, Megan L.; Vitha, Mark F.; Mabbott, Gary A.

    2013-01-01

    High-performance liquid chromatography (HPLC) simulation software has long been recognized as an effective educational tool, yet many of the existing HPLC simulators are either too expensive, outdated, or lack many important features necessary to make them widely useful for educational purposes. Here, a free, open-source HPLC simulator is…

  4. Sorption of catechins under conditions of reverse-phase high-efficiency liquid chromatography

    Science.gov (United States)

    Shafigulin, R. V.; Egorova, K. V.; Bulanova, A. V.

    2010-08-01

    The physico-chemical principles of catechin sorption from various polar solvents onto silica gel modified with octadecyl groups were studied. Thermodynamic characteristics of the sorption were calculated, and the applicability of different models of retention was demonstrated for catechins under the conditions of reverse-phase high-efficiency liquid chromatography.

  5. An on-line high performance liquid chromatography-crocin bleaching assay for detection of antioxidants

    NARCIS (Netherlands)

    Bountagkidou, O.; Klift, van der E.J.C.; Tsimidou, M.Z.; Ordoudi, S.A.; Beek, van T.A.

    2012-01-01

    An on-line HPLC (high performance liquid chromatography) method for the rapid screening of individual antioxidants in mixtures was developed using crocin as a substrate (i.e. oxidation probe) and 2,2'-azobis(2-amidinopropane dihydrochloride (AAPH)) in phosphate buffer (pH 7.5) as a radical generator

  6. DETERMINATION OF ENZYME-ACTIVITY BY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    WELLING, GW; SCHEFFER, AJ; WELLINGWESTER, S

    1994-01-01

    The application of high-performance liquid chromatography (HPLC) in the study of enzymatic reactions is reviewed. The rationale for using HPLC is given and whether the components of the reaction mixture should be derivatized prior to or after HPLC. An alphabetical list of enzymes assayed by HPLC is

  7. Experimental hydrophobicity parameters of perfluorinated alkylated substances from reversed-phase high performance liquid chromatography

    NARCIS (Netherlands)

    de Voogt, P.; Zurano, L.; Serné, P.; Haftka, J.J.H.

    2012-01-01

    Capacity factors of perfluorinated alkylated substances were obtained from isocratic reversed-phase high-performance liquid chromatography-mass spectrometry experiments at different organic modifier strengths of the mobile phase. The resulting capacity factor v. modifier strengths plots were extrapo

  8. Separation of whey proteins for chromatography liquid

    OpenAIRE

    Abraham D. Giraldo Zuñiga; Edwin E.García Rojas; Jane S. R. Coimbra; Wilmer E. Luera Peña

    2010-01-01

    This paper describes and compares three chromatographic methods for the analysis and quantification of most abundant proteins in cheese whey, -lactalbumin and -lactoglobulin. The methods were: Reverse-phase high performance liquid chromatography, anion Exchange chromatography and size-exclusion chromatography. The reverse- phase liquid chromatography led to a better separation of whey proteins than size-exclusion chromatography and anion exchange chromatography, this method offered an excel...

  9. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples.

  10. Surface Confined Ionic Liquid-A New Stationary Phase for the Separation of Ephedrines in High-performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    Shu Juan LIU; Feng ZHOU; Xiao Hua XIAO; Liang ZHAO; Xia LIU; Sheng Xiang JIANG

    2004-01-01

    In this article, a new and effective stationary phase based on ionic liquid modified silica is first reported and used for the separation of ephedrines in high-performance liquid chromatography (HPLC). The separation results indicate the high efficiency and reproducibility of the stationary phase. The electrostatic interaction, ion-exchange interaction between the solutes and the stationary phase are considered to attribute the effective separation. Moreover, the free silanols on the surface of the silica are effectively masked by the immobilized ionic liquid, a result of which is to decrease the non-specific absorption.

  11. Analysis of nitroguanidine in Aqueous Solutions by HPLC (High Performance Liquid Chromatography) with electrochemical Detection and Voltammetry

    Science.gov (United States)

    1987-04-01

    The nitroguanidine was analyzed by high performance liquid chromatography (HPLC) with electrochemical detection at a hanging miercury drop electrode...previously reported on the application of solid sorbent collection techniques to the analysis of several explosives in water by high performance liquid chromatography (HPLC

  12. Dispersive Liquid-Liquid Microextraction and determination of Platinum(IV by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Ali Mazloomifar

    2015-09-01

    Full Text Available A simple, rapid, and efficient procedure, dispersive liquid-liquid microextraction (DLLME, has been developed for the extraction and preconcentration of platinum (IV in environmental water samples. The factors relevant to the microextraction efficiency, such as the kind and volume of extraction and dispersive solvent, the extraction time, the pH in aqueous, and the salt effect, were optimized. Under the optimum conditions , the enrichment factor of this method for platinum was reached at 119. The detection limit for platinum was 0.3 ng mL-1 , and the relative standard deviation (RSD was 0.42% (n = 10 , C = 10 ng mL-1. The method was successfully applied to the determination of trace amounts of platinum in environmental water samples.

  13. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  14. High-throughput, Highly Sensitive Analyses of Bacterial Morphogenesis Using Ultra Performance Liquid Chromatography.

    Science.gov (United States)

    Desmarais, Samantha M; Tropini, Carolina; Miguel, Amanda; Cava, Felipe; Monds, Russell D; de Pedro, Miguel A; Huang, Kerwyn Casey

    2015-12-25

    The bacterial cell wall is a network of glycan strands cross-linked by short peptides (peptidoglycan); it is responsible for the mechanical integrity of the cell and shape determination. Liquid chromatography can be used to measure the abundance of the muropeptide subunits composing the cell wall. Characteristics such as the degree of cross-linking and average glycan strand length are known to vary across species. However, a systematic comparison among strains of a given species has yet to be undertaken, making it difficult to assess the origins of variability in peptidoglycan composition. We present a protocol for muropeptide analysis using ultra performance liquid chromatography (UPLC) and demonstrate that UPLC achieves resolution comparable with that of HPLC while requiring orders of magnitude less injection volume and a fraction of the elution time. We also developed a software platform to automate the identification and quantification of chromatographic peaks, which we demonstrate has improved accuracy relative to other software. This combined experimental and computational methodology revealed that peptidoglycan composition was approximately maintained across strains from three Gram-negative species despite taxonomical and morphological differences. Peptidoglycan composition and density were maintained after we systematically altered cell size in Escherichia coli using the antibiotic A22, indicating that cell shape is largely decoupled from the biochemistry of peptidoglycan synthesis. High-throughput, sensitive UPLC combined with our automated software for chromatographic analysis will accelerate the discovery of peptidoglycan composition and the molecular mechanisms of cell wall structure determination.

  15. Gold nanoparticle decorated graphene oxide/silica composite stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Liang, Xiaojing; Wang, Xusheng; Ren, Haixia; Jiang, Shengxiang; Wang, Licheng; Liu, Shujuan

    2014-06-01

    In the initial phase of this study, graphene oxide (GO)/silica was fabricated by assembling GO onto the silica particles, and then gold nanoparticles (GNPs) were used to modify the GO/silica to prepare a novel stationary phase for high-performance liquid chromatography. The new stationary phase could be used in both reversed-phase chromatography and hydrophilic interaction liquid chromatography modes. Good separations of alkylbenzenes, isomerides, amino acids, nucleosides, and nucleobases were achieved in both modes. Compared with the GO/silica phase and GNPs/silica phase, it is found that except for hydrophilicity, large π-electron systems, hydrophobicity, and coordination functions, this new stationary phase also exhibited special separation performance due to the combination of 2D GO with zero-dimensional GNPs.

  16. Rapid analysis of phentolamine by high-performance liquid chromatography.

    Science.gov (United States)

    Webster, Gregory K; Lemmer, Robert R; Greenwald, Steven

    2003-02-01

    A rapid liquid chromatographic method is validated for the quantitative analysis of phentolamine. Phentolamine exists in three forms for this investigation: as a mesylate salt, hydrochloride salt, and free base. In solution, phentolamine dissociates from its salt and is chromatographed as free phentolamine. This validation confirms the analysis of each form, which is simply based upon molar mass differences encountered in weighing. As such, both the United States Pharmacopeia hydrochloride and mesylate standards are used throughout this validation to demonstrate this equivalency. The validation demonstrates that this method may be used to quantitate phentolamine, regardless of its salt form.

  17. Preparative isolation and analysis of alcohol dehydrogenase inhibitors from Glycyrrhiza uralensis root using ultrafiltration combined with high-performance liquid chromatography and high-speed countercurrent chromatography.

    Science.gov (United States)

    Chen, Miao; Liu, Liangliang; Chen, Xiaoqing

    2014-07-01

    A simple, rapid, and effective assay based on ultrafiltration combined with high-performance liquid chromatography and high-speed countercurrent chromatography was developed for screening and purifying alcohol dehydrogenase inhibitors from Glycyrrhiza uralensis root extract. Experiments were carried out to optimize binding conditions including alcohol dehydrogenase concentration, incubation time, temperature, and pH. By comparing the chromatograms, three compounds were found possessing alcohol dehydrogenase binding activity in Glycyrrhiza uralensis root. Under the target-guidance of ultrafiltration combined with the high-performance liquid chromatography experiment, liquiritin (1), isoliquiritin (2), and liquiritigenin (3) were separated by high-speed countercurrent chromatography using ethyl acetate/methanol/water (5:1:4) as the solvent system. The alcohol dehydrogenase inhibitory activities of these three isolated compounds were assessed; compound 2 showed strongest inhibitory activity with an IC50 of 8.95 μM. The results of the present study indicated that the combinative method using ultrafiltration, high-performance liquid chromatography and high-speed countercurrent chromatography could be widely applied for the rapid screening and isolation of enzyme inhibitors from complex mixtures.

  18. Highly sensitive detection of melamine based on reversed phase liquid chromatography mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    WU QingQing; FAN KeXin; SHA Wei; RUAN HongQiang; ZENG Rong; SHIEH ChiaHui

    2009-01-01

    In this work, we developed a highly sensitive method to detect melamine based on reversed phase liquid chromatography mass spectrometry. A mass spectrometry compatible ion pair, heptafluorobu-tyric acid(HFBA), was used to separate melamine by reversed phase liquid chromatography prior to electrospray mass spectrometry. The incorporation of isotope internal standard and multiple reaction monitoring improved the accuracy and linearity of quantification. Based on this strategy, the method limit of quantification was 0.1 ng/g. The limits of quantification were 8 ng/g for liquid milk and 15 ng/g for dry milk powder. This method provided a reproducible and stable approach to sensitive detection and quantification of melamine.

  19. Effect of high pressure treatment on liquid whole egg

    Science.gov (United States)

    Németh, Csaba; Dalmadi, István; Mráz, Balázs; Friedrich, László; Zeke, Ildikó; Juhász, Réka; Suhajda, Ágnes; Balla, Csaba

    2012-06-01

    In our tests, we artificially infected liquid whole egg samples with Salmonella enteritidis, Listeria monocytogenes, and Staphylococcus aureus bacteria, and then treated the samples in "Food Lab900" high hydrostatic pressure (HHP) instrument for 3-17 min at 200-400 MPa. Subsequently, the change of the viable cell count of the specific bacteria has been tested. In addition to the samples infected with various bacteria, non-infected samples were also treated in each test and the change in viable cell count, colour and viscosity of the samples upon the effect of the treatment. In summary, it can be concluded that in each test of our investigations, the viable cell count of S. enteritidis critical for egg products is reduced significantly, while the reduction of the total viable cell count was around two magnitudes. Additionally, based on our results, microbial destruction, reduction of enthalpy (denaturation of egg white) caused by the treatment at HPP, and colour change are primarily affected by the pressure level, while the changes in rheological properties are also significantly affected by the duration of high pressure treatment (p<0.05).

  20. Determination of chlorobenzenes in textiles by pressurized hot water extraction followed by vortex-assisted liquid-liquid microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lu, Yang; Zhu, Yan

    2013-12-06

    A method for quantitative determination of chlorobenzenes in textiles is developed, using pressurized hot water extraction (PHWE), vortex-assisted liquid-liquid microextraction (VALLME) and gas chromatography-mass spectrometry (GC-MS). VALLME serves as a trapping step after PHWE. The extraction conditions are investigated, as well as the quantitative features such as linearity, limits of detection (LODs), limits of quantification (LOQs), repeatabilities and reproducibilities between days. LOQs of 0.018-0.032mg/kg were achieved. The present method provides good repeatabilities (RSDGC-MS is a simple, rapid and environmentally friendly method for determination of chlorobenzenes in textiles.

  1. Separation of Oligosaccharides from Lotus Seeds via Medium-pressure Liquid Chromatography Coupled with ELSD and DAD

    Science.gov (United States)

    Lu, Xu; Zheng, Zhichang; Miao, Song; Li, Huang; Guo, Zebin; Zhang, Yi; Zheng, Yafeng; Zheng, Baodong; Xiao, Jianbo

    2017-03-01

    Lotus seeds were identified by the Ministry of Public Health of China as both food and medicine. One general function of lotus seeds is to improve intestinal health. However, to date, studies evaluating the relationship between bioactive compounds in lotus seeds and the physiological activity of the intestine are limited. In the present study, by using medium pressure liquid chromatography coupled with evaporative light-scattering detector and diode-array detector, five oligosaccharides were isolated and their structures were further characterized by electrospray ionization-mass spectrometry and gas chromatography-mass spectrometry. In vitro testing determined that LOS3-1 and LOS4 elicited relatively good proliferative effects on Lactobacillus delbrueckii subsp. bulgaricus. These results indicated a structure-function relationship between the physiological activity of oligosaccharides in lotus seeds and the number of probiotics applied, thus providing room for improvement of this particular feature. Intestinal probiotics may potentially become a new effective drug target for the regulation of immunity.

  2. Quality Evaluation of Potentilla fruticosa L. by High Performance Liquid Chromatography Fingerprinting Associated with Chemometric Methods

    OpenAIRE

    Wei Liu; Dongmei Wang; Jianjun Liu; Dengwu Li; Dongxue Yin

    2016-01-01

    The present study was performed to assess the quality of Potentilla fruticosa L. sampled from distinct regions of China using high performance liquid chromatography (HPLC) fingerprinting coupled with a suite of chemometric methods. For this quantitative analysis, the main active phytochemical compositions and the antioxidant activity in P. fruticosa were also investigated. Considering the high percentages and antioxidant activities of phytochemicals, P. fruticosa samples from Kangding, Sichua...

  3. Resolution of the stereoisomers of baclofen by high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Weatherby, R.P.; Allan, R.D.; Johnston, G.A.R. (Sydney Univ. (Australia))

    1984-01-01

    The GABA analogue baclofen (3-(p-chlorophenyl)-4-aminobutanoic acid) has stereospecific actions on the peripheral and central nervous systems. This paper describes the resolution of tritium-labelled baclofen by high performance liquid chromatography on a reverse-phase C18 column using a chiral mobile phase. The method, which may have general application to certain other GABA analogues, affords optically pure (+)- and (-)-baclofen labelled with tritium to high specific activity suitable for ligand binding and other neurochemical studies.

  4. Determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry

    Science.gov (United States)

    Hostetler, K.A.; Thurman, E.M.

    2000-01-01

    Analytical methods using high-performance liquid chromatography-diode array detection (HPLC-DAD) and high-performance liquid chromatography/mass spectrometry (HPLC/MS) were developed for the analysis of the following chloroacetanilide herbicide metabolites in water: alachlor ethanesulfonic acid (ESA); alachlor oxanilic acid; acetochlor ESA; acetochlor oxanilic acid; metolachlor ESA; and metolachlor oxanilic acid. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The average HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.5 and 2.0 ??g/l ranged from 84 to 112%, with relative standard deviations of 18% or less. The average HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.2 and 2.0 ??g/l ranged from 81 to 118%, with relative standard deviations of 20% or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 ??g/l, whereas the LOQ using the HPLC/MS method was at 0.05 ??g/l. These metabolite-determination methods are valuable for acquiring information about water quality and the fate and transport of the parent chloroacetanilide herbicides in water. Copyright (C) 2000 Elsevier Science B.V.

  5. Chemical fingerprint of Ganmaoling granule by double-wavelength ultra high performance liquid chromatography and ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Lou, Qiong; Ye, Xiaolan; Zhou, Yingyi; Li, Hua; Song, Fenyun

    2015-06-01

    A method incorporating double-wavelength ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry was developed for the investigation of the chemical fingerprint of Ganmaoling granule. The chromatographic separations were performed on an ACQUITY UPLC HSS C18 column (2.1 × 50 mm, 1.8 μm) at 30°C using gradient elution with water/formic acid (1%) and acetonitrile at a flow rate of 0.4 mL/min. A total of 11 chemical constituents of Ganmaoling granule were identified from their molecular weight, UV spectra, tandem mass spectrometry data, and retention behavior by comparing the results with those of the reference standards or literature. And 25 peaks were selected as the common peaks for fingerprint analysis to evaluate the similarities among 25 batches of Ganmaoling granule. The results of principal component analysis and orthogonal projection to latent structures discriminant analysis showed that the important chemical markers that could distinguish the different batches were revealed as 4,5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4-O-caffeoylquinic acid. This is the first report of the ultra high performance liquid chromatography chemical fingerprint and component identification of Ganmaoling granule, which could lay a foundation for further studies of Ganmaoling granule.

  6. Determination of 1-hydroxypyrene in human urine by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Poulsen, O M; Christensen, J M

    1993-01-01

    A high-performance liquid chromatography (HPLC)/fluorescence method for quantitative analysis of 1-hydroxypyrene in urine was developed. The method validation analysis showed the method to be in analytical control. No significant systematical errors could be demonstrated. The entire run time...... of chromatography was 10 min using isocratic elution (acetonitrile-water, 70:30), and the retention time for 1-hydroxypyrene was 3.5 min. The short run time in combination with the low limit detection (1.37 nmol/L) makes the method potentially applicable for surveillance of pyrene exposure in work environments...

  7. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    C.J. Miller; G. Elias; N.C. Schmitt; C. Rae

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to specifically identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol using no sample cleanup prior to analysis. The methanol extracts were injected directly into several different column types and analyzed by HPLC-UV and/or GC-ECD. This paper describes general screening methods that were used to determine the presence of explosives in unknown samples and techniques that have been optimized for quantification of each explosive from the substrate extracts.

  8. Determination of five antiarrhythmic drugs in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Jouyban, Abolghasem; Sorouraddin, Mohammad Hossein; Farajzadeh, Mir Ali; Somi, Mohammad Hossein; Fazeli-Bakhtiyari, Rana

    2015-03-01

    A fast and sensitive high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection was developed and validated for the simultaneous quantitation of five antiarrhythmic drugs (metoprolol, propranolol, carvedilol, diltiazem, and verapamil) in human plasma samples. It involves dispersive liquid-liquid microextraction (DLLME) of the desired drugs from 660 µL plasma and separation using isocratic elution with UV detection at 200 nm. The complete separation of all analytes was achieved within 7 min. Acetonitrile (as disperser solvent) resulting from the protein precipitation procedure was mixed with 100 µL dichloromethane (as an extraction solvent) and rapidly injected into 5 mL aqueous solution (pH 11.5) containing 1% (w/v), NaCl. After centrifugation, the sedimented phase containing enriched analytes was collected and evaporated to dryness. The residue was re-dissolved in 50 µL de-ionized water (acidified to pH 3) and injected into the HPLC system for analysis. Under the optimal conditions, the enrichment factors and extraction recoveries ranged between 4.4-10.8 and 33-82%, respectively. The suggested method was linear (r(2) ≥0.997) over a dynamic range of 0.02-0.80 µg mL(-1) in plasma. The intra- and inter-days relative standard deviation (RSD%) and relative error (RE%) values of the method were below 20%, which shows good precision and accuracy. Finally, this method was applied to the analysis of real plasma samples obtained from the patients treated with these drugs.

  9. Analysis of drugs of abuse in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Fernández, P; Regenjo, M; Bermejo, A M; Fernández, A M; Lorenzo, R A; Carro, A M

    2015-04-01

    Opioids and cocaine are widely used at present, both for recreational purposes and as drugs of abuse. This raises the need to develop new analytical methods specifically designed for the simultaneous detection of several drugs of abuse in biological samples. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a new sample treatment for the simultaneous extraction of morphine (MOR), 6-acetylmorphine (6AM), cocaine (COC), benzoylecgonine (BZE) and methadone (MET) from human plasma. Preliminary assays were done before developing an experimental design based on a Uniform Network Doehlert which allowed the optimum extraction conditions to be identified, namely: a volume of extractant solvent (chloroform) and dispersant solvent (acetonitrile) of 220 µl and 3.2 ml, respectively; 0.2 g of NaCl as a salting-out additive; pH 10.6 and ultrasound stirring for 3.5 min. The resulting extracts were analyzed by high-performance liquid chromatography with photodiode array detection (HPLC-PDA), using an XBridge® RP18 column (250 × 4.6 mm i.d., 5 µm particle size). Calibration graphs were linear over the concentration range 0.1-10 µg ml⁻¹, and detection limits ranged from 13.9 to 28.5 ng ml⁻¹. Precision calculated at three different concentration levels in plasma was included in the range 0.1-6.8% RSD. Recoveries of the five drugs were all higher than 84% on average. Finally the proposed method was successfully applied to 22 plasma samples from heroin, cocaine and/or methadone users, and the most frequently detected drug was benzoylecgonine, followed by methadone, cocaine and morphine.

  10. Analyses of acute kidney injury biomarkers by ultra-high performance liquid chromatography with mass spectrometry.

    Science.gov (United States)

    Al Za'abi, Mohammed; Ali, Badreldin H; ALOthman, Zeid A; Ali, Imran

    2016-01-01

    The newly developed acute kidney injury biomarkers are very important for the early and timely detection of kidney diseases. This review contains details of the analyses of several acute kidney injury biomarkers using ultra-high performance liquid chromatography-mass spectrometry in urine and plasma samples. In this review we attempt to discuss some aspects of the types of the biomarkers, patents, sample preparation, and the analyses. Besides, efforts were also made to discuss the possible uses of superficially porous (core-shell) columns in traditional and inexpensive high-performance liquid chromatography instruments. Additionally, the challenges and the future prospects are also highlighted. The present review will be useful for the academicians, scientists, and clinicians for the early detection of acute kidney injury biomarkers.

  11. Homochiral metal-organic framework used as a stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Kong, Jiao; Zhang, Mei; Duan, Ai-Hong; Zhang, Jun-Hui; Yang, Rui; Yuan, Li-Ming

    2015-02-01

    Metal-organic frameworks are promising porous materials. Chiral metal-organic frameworks have attracted considerable attention in controlling enantioselectivity. In this study, a homochiral metal-organic framework [Co(2) (D-cam)(2) (TMDPy)] (D-cam = D-camphorates, TMDPy = 4,4'-trimethylenedipyridine) with a non-interpenetrating primitive cubic net has been used as a chiral stationary phase in high-performance liquid chromatography. It has allowed the successful separation of six positional isomers and six chiral compounds. The good selectivity and baseline separation, or at least 60% valley separation, confirmed its excellent molecular recognition characteristics. The relative standard deviations for the retention time of run-to-run and column-to-column were less than 1.8 and 3.1%, respectively. These results demonstrate that [Co(2) (D-cam)(2) (TMDPy)] may represent a promising chiral stationary phase for use in high-performance liquid chromatography.

  12. Serum Protein Profile Study of Clinical Samples Using High Performance Liquid Chromatography-Laser Induced Fluorescence

    DEFF Research Database (Denmark)

    Karemore, Gopal Raghunath; Ukendt, Sujatha; Rai, Lavanya

    2009-01-01

    The serum protein profiles of normal subjects, patients diagnosed with cervical cancer, and oral cancer were recorded using High Performance Liquid Chromatography combined with Laser Induced Fluorescence detection (HPLC-LIF). Serum protein profiles of the above three classes were tested for estab......The serum protein profiles of normal subjects, patients diagnosed with cervical cancer, and oral cancer were recorded using High Performance Liquid Chromatography combined with Laser Induced Fluorescence detection (HPLC-LIF). Serum protein profiles of the above three classes were tested...... for establishing the ability of HPLC-LIF protein profiling technique for discrimination, using hard clustering and Fuzzy clustering methods. The clustering algorithms have quite successfully classified the profiles as belonging to normal, cancer of cervix, and oral cancer conditions....

  13. Chemical Investigation of Saponins in Different Parts of Panax notoginseng by Pressurized Liquid Extraction and Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Si-Jia Hong

    2012-05-01

    Full Text Available A pressurized liquid extraction (PLE and high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS method was developed for the qualitative determination of saponins in different parts of P. notoginseng, including rhizome, root, fibre root, seed, stem, leaf and flower. The samples were extracted using PLE. The analysis was achieved on a Zorbax SB-C18 column with gradient elution of acetonitrile and 8 mM aqueous ammonium acetate as mobile phase. The mass spectrometer was operated in the negative ion mode using the electrospray ionization, and a collision induced dissociation (CID experiment was also carried out to aid the identification of compounds. Forty one saponins were identified in different parts of P. notoginseng according to the fragmentation patterns and literature reports, among them, 21 saponins were confirmed by comparing the retention time and ESI-MS data with those of standard compounds. The results showed that the chemical characteristics were obviously diverse in different parts of P. notoginseng, which is helpful for pharmacological evaluation and quality control of P. notoginseng.

  14. Quantification of furanic derivatives in fortified wines by a highly sensitive and ultrafast analytical strategy based on digitally controlled microextraction by packed sorbent combined with ultrahigh pressure liquid chromatography.

    Science.gov (United States)

    Perestrelo, Rosa; Silva, Catarina L; Câmara, José S

    2015-02-13

    An improved, reliable and powerful analytical strategy based on digitally controlled microextraction by packed sorbent (MEPS) combined with ultrahigh pressure liquid chromatography (UHPLC) was validated for the simultaneous identification and quantification of major furanic derivatives, namely 5-hydroxymethyl-2-furaldehyde (5HMF), 5-methyl-2-furaldehyde (5MF), 2-furaldehyde (2F) and 2-furyl methyl ketone (2FMK), in fortified wines. To enhance the extraction efficiency of the target furanic derivates, several influencing extraction parameters, such as number of loading cycles, nature of elution solvent and elution volume, were evaluated and optimized. In addition the ability of different MEPS sorbent materials, namely C2, C8, C18, SIL, M1, R-AX, R-CX and PGC, were also tested. The optimal analytical conditions involved loading 3×200 μL of wine samples through a C8 sorbent in a MEPS syringe placed in the semi-automatic eVolH syringe followed by elution using 200 μL MeOH:H2O (95:5, v/v). The furanic derivates separation was achieved using a CORTECS UPLC(®) C18 analytical column in an ultrafast chromatographic run (within 4 min). The method performance was assessed for dry/medium dry (D/MD) and sweet/medium sweet (S/MS) model wines in terms of selectivity, linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision and matrix effect, using model wine matrix-matched calibration. Good linearity was obtained with a regression coefficient (r(2)) higher than 0.992. A good precision was attained (RSDquantification limits (LOQ) for D/MD model wines ranged from 14.9 to 431.0 ng L(-1), whereas for S/MS model wines range from 23.1 to 950.5 ng L(-1). The method also afforded satisfactory results in terms of accuracy, ranging from 74 to 97% for D/MD wines and between 84 and 99% for S/MS wines. The MEPS(C8)/UHPLC-PDA analytical strategy was successfully applied to analyze furanic derivates in 26 fortified Madeira wines from different types (D/MD, S

  15. Rapid determination of pesticide residues in herbs using selective pressurized liquid extraction and fast gas chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Du, Gang; Xiao, Yao; Yang, Hua-Rong; Wang, Li; Song, Yue-Lin; Wang, Yi-Tao

    2012-08-01

    A selective pressurized liquid extraction and gas chromatography coupled with triple quadrupole mass spectrometer method was developed for simultaneous determination of 52 pesticide residues in medicine and food dual-purpose herbs. The developed extraction method integrated extraction and cleanup processes for sample preparation. The sorbents, 5 g Florisil and 100 mg graphitized carbon black, were placed inside the extraction cell to remove matrix interferences. Optimized conditions of selective pressurized liquid extraction were ethyl acetate as extraction solvent, 120°C of extraction temperature, 6 min of static extraction time, 50% of flush volume extracted for two cycles. An ultra inert capillary GC-MS HP-5 UI column (20 m × 0.18 mm id, 0.18 μm) and column backflush system were used for the analysis. Multiple-reaction monitoring was employed for the quantitative analysis with electron ionization mode. All calibration curves showed good linearity (r(2) > 0.995) within the test ranges. The average recoveries of most pesticides were from 81 to 118%. The validated method was successfully applied for the determination of pesticide residues in four herbs. The results indicate that selective pressurized liquid extraction and GC-MS/MS is a sensitive and reliable analytical method for the simultaneous determination of multiple pesticide residues in herbs.

  16. [Comparison of refractometric and ultraviolet detection methods in lactulose assay by high performance liquid chromatography].

    Science.gov (United States)

    Vaccher, C; Berthelot, P; Flouquet, N; Debaert, M

    1990-01-01

    Dosage of lactulose and determination of related sugars (lactose, fructose, galactose, épilactose) were undertaken by high performance liquid chromatography (HPLC). The present note described two modes of detection used simultaneously and compared: refractive index detector (RI) and multiwavelength ultraviolet detector (UV). HPLC is performed with an aminopropylsylil phase as stationary phase and an isocratic mobile phase containing acetonitrile and aqueous sodium phosphate. The results are outlined and discussed.

  17. Isolation and purification of heroin from heroin street samples by preparative high performance liquid chromatography.

    Science.gov (United States)

    Guo, Zhen; Zheng, Hui; Lu, Yanzhen; Wei, Yun

    2012-09-10

    The present study established a novel method using preparative high performance liquid chromatography to isolate and purify heroin·HCl from heroin street samples to be used as a reference standard. Different kinds of mobile phases and columns were used, ultimately the mobile phase consisting of hexane-isopropanol-methanol (65:28:7, v/v) and the SIL preparative column prepared in laboratory were selected as the final condition. Heroin was further purified by the drowning-out crystallization method using isopropanol-methanol (50:1, v/v) and hexane as drowning-out anti-solvents and salting-out agents, respectively. The purity was assessed by analytical high performance liquid chromatography and the confirmation of the chemical structure was performed by IR and NMR. About 110.7mg of heroin·HCl at a purity of over 99.52% was obtained from 180mg of heroin street samples which contained 156.15mg of heroin·HCl component by preparative high performance liquid chromatography. This method is suitable for preparing heroin standards in forensic science area.

  18. Fractionation of Gibberellins in plant extracts by reverse phase high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Jones, M.G.; Metzger, J.D.; Zeevaart, J.A.D.

    1980-02-01

    In studies on endogenous plant gibberellins (GAs), reverse phase (Bondapak C/sub 18/) high performance liquid chromatography (HPLC) has proved to be a useful method for the fractionation of plant extracts. The behavior of 18 authentic GAs in such a chromatographic system is described. The main factors determining chromatographic behavior are the degree and the position of hydroxylation of the GA. As an illustration of the use of reverse phase HPLC, the endogeneous GAs of immature seeds of Pharbitis nil L., strain Violet, were reinvestigated. The presence of gibberellins A/sub 3/, A/sub 5/, A/sub 17/, A/sub 20/, and A/sub 29/ was confirmed by gas-liquid chromatography-mass spectrometry. In addition, two other GAs, A/sub 19/ and A/sub 44/, were also identified in extracts of this material.

  19. Determination of muscimol and ibotenic acid in Amanita mushrooms by high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tsujikawa, Kenji; Kuwayama, Kenji; Miyaguchi, Hajime; Kanamori, Tatsuyuki; Iwata, Yuko; Inoue, Hiroyuki; Yoshida, Takemi; Kishi, Tohru

    2007-06-01

    A reliable analytical method was developed for the quantification and identification of muscimol (MUS) and ibotenic acid (IBO), the toxic constituents of Amanita muscaria and Amanita pantherina. MUS and IBO were extracted from mushrooms by aqueous methanol and derivatized with dansyl chloride (DNS-Cl). After extraction with ethyl acetate and evaporation of the solvent, the residue was ethylated with 1.25 M hydrogen chloride in ethanol. The resulting derivatives were quantified by high-performance liquid chromatography with UV detection and identified by liquid chromatography electrospray ionization tandem mass spectrometry. Calibration curves were linear in the range of 25-2500 ppm for MUS and 40-2500 ppm for IBO, respectively. This method was successfully applied to identify and quantify MUS and IBO in Amanita mushrooms naturally grown and circulated in the drug market.

  20. Recent advances in ultra-high performance liquid chromatography for the analysis of traditional chinese medicine

    Science.gov (United States)

    Traditional Chinese medicines (TCMs) have been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra Performance Liquid Chromatography (UHPLC) is a relatively new technique offering new possibilities in liquid chromatography. This paper reviews recen...

  1. Applications of nanomaterials in liquid chromatography: opportunities for separation with high efficiency and selectivity.

    Science.gov (United States)

    Zhang, Zhengxiang; Wang, Zhiyong; Liao, Yiping; Liu, Huwei

    2006-08-01

    During recent decades, great efforts have been made to improve the chemical stability, selectivity, and separation efficiency of stationary phases in liquid chromatography. Significant progress has been achieved, especially after the introduction of nanomaterials into separation science. This review covers the applications of nanomaterials playing various roles in liquid chromatography. Future possibilities for developing nanomaterial-based stationary phases are also discussed.

  2. Ultrasound-assisted ionic liquid-based homogeneous liquid-liquid microextraction high-performance liquid chromatography for determination of tanshinones in Salvia miltiorrhiza Bge. root.

    Science.gov (United States)

    Wang, Zhibing; Cao, Bocheng; Yu, Aimin; Zhang, Hanqi; Qiu, Fangping

    2015-02-01

    The ultrasound-assisted ionic liquid-based homogeneous liquid-liquid microextraction has been developed and applied to the extraction of four tanshinones, including dihydrotanshinone, tanshinone I, cryptotanshinone and tanshinone IIA in Salvia miltiorrhiza Bge. root. High performance liquid chromatography was applied to the separation and determination of the analytes. The ionic liquid was used as extraction solvent and target analytes were extracted with help of ultrasound. Then, ion-pairing agent was added into the sample solution, which resulted in the formation of water-insoluble ionic liquid in the solution. The phase separation was performed by centrifugation. The extraction, concentration and purification of target analytes were performed simultaneously. The experimental parameters, including type and volume of ionic liquid, sample amount, the size of sample particle, pH value of extraction medium, extraction temperature, extraction time, amount of ion-pairing agent and centrifuging time, were investigated and optimized. The calibration curves showed good linear relationship (r>0.9997). The limits of detection and quantification were in the range of 0.052-0.093 and 0.17-0.31 μg mL(-1), respectively. The recoveries were between 70.45% and 94.23% with relative standard deviations lower than 5.31%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with UAE and HRE. There was no obvious difference in the extraction yields of active constitutions obtained by the three extraction methods.

  3. Ultra high performance liquid chromatography versus high performance liquid chromatography: stationary phase selectivity for generic carotenoid screening.

    Science.gov (United States)

    Bijttebier, Sebastiaan; D'Hondt, Els; Noten, Bart; Hermans, Nina; Apers, Sandra; Voorspoels, Stefan

    2014-03-07

    Aim of study was to find the most suitable LC column for generic carotenoid screening. To represent the diversity of carotenoids in nature and to optimize chromatographic separation, a set of carotenoid standards was carefully chosen to account for the various classes of carotenoids. The HPLC C30 column has since long been the 'golden standard' in the chromatographic separation of carotenoids. Since approximately one decade, new UHPLC technology has led to much shorter analysis times, smaller peak widths and higher chromatographic resolution. However, there are currently no UHPLC columns on the market containing the specific stationary phase chemistry of the HPLC C30 column. Therefore during this study, we investigated the separation of carotenoids on a set of UHPLC columns and compared it to their separation on the HPLC C30 column. Comparison of carotenoids separations on the different stationary phases with objective column comparison parameters clearly indicated that the HPLC C30 column is an overall better performer in the separation of carotenoids. This is due to the lack of UHPLC column chemistries that are adapted for carotenoid analysis. However, analysis time on the HPLC C30 column takes about four times longer compared to UHPLC analysis. Therefore, with the range of columns that are commercially available nowadays, a choice has to be made between very high selectivity (HPLC C30 column) and analysis times that are adapted to modern laboratory requirements (UHPLC technology). Therefore, carotenoid separations would be even more performing if an appropriate UHPLC C30 column would be available.

  4. [Qualitative and quantitative analysis of the amino acids in Rhizoma Arisaematis by ultra high performance liquid chromatography-tandem mass spectrometry and high performance liquid chromatography].

    Science.gov (United States)

    Wang, Xing; Chi, Yumei; Kang, An

    2014-12-01

    A method for the identification and determination of the polar amino components without ultraviolet activity in traditional Chinese medicines was developed. With Rhizoma Arisaematis as the object of this study, using pre-column derivatization with phenyl isothiocyanate (PITC) as the derivatization reagent, compounds were separated and identified on a C18 column (100 mm x 2.1 mm, 3.5 µm) by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A total of 20 components, including 18 amino acids and 2 amine compounds were identified. Furthermore, after the optimization of the derivatization conditions, 15 amino acids were determined by high performance liquid chromatography (HPLC) on Diamonsil C18 column (250 mm x 4.6 mm, 5 µm), detected at 254 nm and gradiently eluted by acetonitrile and 0. 05 mol/L ammonium acetate-acetic acid (pH 6. 5) as the mobile phases. The results of methodological study demonstrated that the method can meet the requirements of the determination. All calibration curves expressed good linearity: Glu, Try in the range of 2-100 mg/L, Arg in the range of 6-300 mg/L, others in the range of 0. 8-40 µg/L, with the correlation coefficients ≥ 0. 999 5. The average recovery of this method was among 95%-105% and the RSD was less than 3%. The developed method was successfully applied to quantitative determination of amino compounds in 12 batches of Rhizoma Arisaematis samples. The method is simple, sensitive, accurate, and can be used for rapid identification and determination of amino components in traditional Chinese medicines.

  5. Surveillance of the Army’s Propellant Stockpile: Analysis of Stabilizer Content by High Performance Liquid Chromatography

    Science.gov (United States)

    1990-10-01

    high performance liquid chromatography to monitor the level of stabilizer and its daughter products in propellant. Three of those methods are presented along with statistics and some comments about their

  6. High performance liquid chromatography-mass spectrometry analysis of high antioxidant australian fruits with antiproliferative activity against cancer cells

    Directory of Open Access Journals (Sweden)

    Joseph Sirdaarta

    2016-01-01

    Abbreviations used: DPPH: di (phenyl- (2,4,6-trinitrophenyl iminoazanium, HPLC: High-performance liquid chromatography, IC50: The concentration required to inhibit by 50%, LC50: The concentration required to achieve 50% mortality, MS: Mass spectrometry. Ian Edwin Cock

  7. High-performance liquid chromatography-mass spectrometry analysis of plant metabolites in brassicaceae.

    Science.gov (United States)

    De Vos, Ric C H; Schipper, Bert; Hall, Robert D

    2012-01-01

    The Brassicaceae family comprises a variety of plant species that are of high economic importance as -vegetables or industrial crops. This includes crops such as Brassica rapa (turnip, Bok Choi), B. oleracea (cabbages, broccoli, cauliflower, etc.), and B. napus (oil seed rape), and also includes the famous genetic model of plant research, Arabidopsis thaliana (thale cress). Brassicaceae plants contain a large variety of interesting secondary metabolites, including glucosinolates, hydroxycinnamic acids, and flavonoids. These metabolites are also of particular importance due to their proposed positive effects on human health. Next to these well-known groups of phytochemicals, many more metabolites are of course also present in crude extracts prepared from Brassica and Arabidopsis plant material.High-pressure liquid chromatography coupled to mass spectrometry (HPLC-MS), especially if combined with a high mass resolution instrument such as a QTOF MS, is a powerful approach to separate, detect, and annotate metabolites present in crude aqueous-alcohol plant extracts. Using an essentially unbiased procedure that takes into account all metabolite mass signals from the raw data files, detailed information on the relative abundance of hundreds of both known and, as yet, unknown semipolar metabolites can be obtained. These comprehensive metabolomics data can then be used to, for instance, identify genetic markers regulating metabolic composition, determine effects of (a)biotic stress or specific growth conditions, or establish metabolite changes occurring upon food processing or storage.This chapter describes in detail a procedure for preparing crude extracts and performing comprehensive HPLC-QTOF MS-based profiling of semi-polar metabolites in Brassicaceae plant material. Compounds present in the extract can be (partially or completely) annotated based on their accurate mass, their MS/MS fragments and on other specific chemical characteristics such as retention time and UV

  8. Ultrapressure liquid chromatography-tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for quantification of 4-methoxydiphenylmethane in pharmacokinetic evaluation.

    Science.gov (United States)

    Farhan, Nashid; Fitzpatrick, Sean; Shim, Yun M; Paige, Mikell; Chow, Diana Shu-Lian

    2016-09-05

    4-Methoxydiphenylmethane (4-MDM), a selective augmenter of Leukotriene A4 Hydrolase (LTA4H), is a new anti-inflammatory compound for potential treatment of chronic obstructive pulmonary disease (COPD). Currently, there is no liquid chromatography tandem mass spectrometric (LC-MS/MS) method for the quantification of 4-MDM. A major barrier for developing the LC-MS/MS method is the inability of electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) to ionize 4-MDM due to its hydrophobicity and lack of any functional group for ionization. With the advent of atmospheric pressure photoionization (APPI) technique, many hydrophobic compounds have been demonstrated to ionize by charge transfer reactions. In this study, a highly sensitive ultrapressure liquid chromatography tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for the quantifications of 4-MDM in rat plasma has been developed and validated. 4-MDM was extracted from the plasma by solid phase extraction (SPE) and separated chromatographically using a reverse phase C8 column. The photoionization (PI) was achieved by introducing anisole as a dopant to promote the reaction of charge transfer. The assay with a linear range of 5 (LLOQ)-400ngmL(-1) met the regulatory requirements for accuracy, precision and stability. The validated assay was employed to quantify the plasma concentrations of 4-MDM after an oral dosing in Sprague Dawley (SD) rats.

  9. Quantitative determination of acetylcholine in microdialysis samples using liquid chromatography/atmospheric pressure spray ionization mass spectrometry.

    Science.gov (United States)

    Keski-Rahkonen, Pekka; Lehtonen, Marko; Ihalainen, Jouni; Sarajärvi, Timo; Auriola, Seppo

    2007-01-01

    A fast, simple and sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for the determination of acetylcholine in rat brain microdialysis samples. The chromatographic separation was achieved in 3 min on a reversed-phase column with isocratic conditions using a mobile phase containing 2% (v/v) of acetonitrile and 0.05% (v/v) of trifluoroacetic acid (TFA). A stable isotope-labeled internal standard was included in the analysis and detection was carried out with a linear ion trap mass spectrometer using selected reaction monitoring (SRM). Analyte ionization was performed with an atmospheric pressure chemical ionization (APCI) source without applying discharge current (atmospheric pressure spray ionization). This special ionization technique offered significant advantages over electrospray ionization for the analysis of acetylcholine with reversed-phase ion-pairing chromatography. The lower limit of quantification was 0.15 nM (1.5 fmol on-column) and linearity was maintained over the range of 0.15-73 nM, providing a concentration range that is significantly wider than that of the existing LC/MS methods. Good accuracy and precision were obtained for concentrations within the standard curve range. The method was validated and has been used extensively for the determination of acetylcholine in rat brain microdialysis samples.

  10. Studies on Chromatography Fingerprint of Hongqi by High-performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    Shi Lan FENG; Fang Di HU; Jian Xiong ZHAO; Jing Wen XU; Li Ren CHEN

    2004-01-01

    Chromatography fingerprint (CFP) of 10 samples of hongqi were studied. 23 common peaks were analyzed, their average similarity was 97.29%. CFP were positioned with main index composition such as formononetin, calycosin and then the contents of index composition were determined. The character and exclusive of CFP of 10 samples of hongqi were clear. CFP and content determination of index composition of hongqi could be used to evaluate the quality of hongqi comprehensively.

  11. Microwave-assisted ionic liquid homogeneous liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of anthraquinones in Rheum palmatum L.

    Science.gov (United States)

    Wang, Zhibing; Hu, Jianxue; Du, Hongxia; He, Shuang; Li, Qing; Zhang, Hanqi

    2016-06-01

    The microwave-assisted ionic liquid homogeneous liquid-liquid microextraction (MA-IL-HLLME) coupled with high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones, including aloe-emodin, emodin, chrysophanol and physcion in root of Rheum palmatum L. Several experimental parameters influencing the extraction efficiency, including amount of sample, type and volume of ionic liquid, volume and pH value of extraction medium, microwave power and extraction time, concentration of NH4PF6 as well as centrifugal condition were optimized. When 140μL of ionic liquid ([C8MIM][BF4]) was used as an extraction solvent, target analytes can be extracted from sample matrix in one minute with the help of microwave irradiation. The MA-IL-HLLME is simple and quick. The calibration curves exhibited good linear relationship (r>0.9984). The limits of detection and quantification were in the range of 0.015-0.026 and 0.051-0.088μgmL(-1), respectively. The spiked recovery for each analyte was in the range of 81.13-93.07% with relative standard deviations lower than 6.89%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with ultrasonic and heat reflux extraction. The results indicated that the present method can be successfully applied to the determination of anthraquinones in medicinal plant.

  12. [Determination of five triazine herbicides in infant milk powder by high performance liquid chromatography coupled with ionic liquid-based homogeneous liquid-liquid microextraction].

    Science.gov (United States)

    Zhang, Liyuan; Yao, Di; Li, Na; Zhang, Hanqi; Yu, Aimin

    2015-07-01

    A high performance liquid chromatography coupled with homogeneous liquid-liquid microextraction was developed for the determination of five triazine herbicides in infant milk powders. The ionic liquid was used as microextraction solvent. The separation of the herbicides was performed on an Eclipse XDB-C18 column using acetonitrile and water as mobile phases in gradient mode. The effects of homogeneous liquid-liquid extraction conditions on the experimental results were investigated in detail. Under the optimized experimental conditions, the calibration curves for determining the analytes were linear and the correlation coefficients were ≥ 0.9992. The limits of detection for cyanazine, desmetryn, terbumeton, terbuthylazine and dimethametryn were 12.1, 13.8, 11.8, 14.6 and 13.7 μg/kg, respectively. The recoveries of the analytes spiked in four infant milk powders ranged from 92.2% to 103.2% and the relative standard deviations were lower than 6%. This method is sensitive, simple, and suitable for the determination of triazine herbicides in milk powder samples.

  13. Micellar liquid chromatography

    Science.gov (United States)

    Basova, Elena M.; Ivanov, Vadim M.; Shpigun, Oleg A.

    1999-12-01

    Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

  14. Preliminary Validation of High Performance Liquid Chromatography Method for Detection of Methyltestosterone Residue in Carp Muscle

    Institute of Scientific and Technical Information of China (English)

    JIANG Jie; LIN Hong; FU Xiaoting; LI Mingming

    2005-01-01

    The use of synthetic anabolic steroid methyltestosterone (MT) as growth promoter is prohibited in China. Validations of analytical methods for MT residue in food and the results obtained have become indispensable. The high performance liquid chromatography (HPLC) method for the detection of MT with liquid-liquid extraction by trichloromethanemethanol in carp muscle tissue was preliminarily validated with reference to the following parameters: recovery (accuracy)at the 1, 5 and 10 mgkg-1 level, between-run and within-run CV values (repeatability, also called relative standard deviation(RSD)) and limit of detection. The recoveries were above 80% and the between-run and within-run CV values below 10%for muscle tissue. The limit of detection was 0.05 mgkg-1.

  15. Transport properties of liquid metal hydrogen under high pressures

    Science.gov (United States)

    Brown, R. C.; March, N. H.

    1972-01-01

    A theory is developed for the compressibility and transport properties of liquid metallic hydrogen, near to its melting point and under high pressure. The interionic force law is assumed to be of the screened Coulomb type, because hydrogen has no core electrons. The random phase approximation is used to obtain the structure factor S(k) of the system in terms of the Fourier transform of this force law. The long wavelenth limit of the structure factor S(o) is related to the compressibility, which is much lower than that of alkali metals at their melting points. The diffusion constant at the melting point is obtained in terms of the Debye frequency, using a frequency spectrum analogous with the phonon spectrum of a solid. A similar argument is used to obtain the combined shear and bulk viscosities, but these depend also on S(o). The transport coefficients are found to be about the same size as those of alkali metals at their melting points.

  16. Preparation and Characterization of a Polymeric Monolithic Column for Use in High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Bindis, Michael P.; Bretz, Stacey Lowery; Danielson, Neil D.

    2011-01-01

    The high-performance liquid chromatography (HPLC) experiment, most often done in the undergraduate analytical instrumentation laboratory course, generally illustrates reversed-phase chromatography using a commercial C[subscript]18 silica column. To avoid the expense of periodic column replacement and introduce a choice of columns with different…

  17. tRNA separation by high-performance liquid chromatography using an aggregate of ODS-Hypersil and trioctylmethylammonium chloride

    NARCIS (Netherlands)

    Bischoff, Rainer; Graeser, E.; Mclaughlin, L.W.

    1983-01-01

    High-performance liquid chromatography on a reversed-phase support treated with a tetraalkylammonium salt was used to separate tRNAs from baker's yeast. While resolution by this column appears to result from both anion-exchange and reversed-phase chromatography, it is the hydrophobic interactions wh

  18. Ultra high efficiency/low pressure supercritical fluid chromatography with superficially porous particles for triglyceride separation.

    Science.gov (United States)

    Lesellier, E; Latos, A; de Oliveira, A Lopes

    2014-01-31

    This paper reports the development of the separation of vegetable oil triglycerides (TG) in supercritical chromatography (SFC), using superficially porous particles (SPPs). The SPP, having a small diameter (2-3μm), provide a higher theoretical plate number (N), which allows to improve separation of critical pairs of compounds. However, compared to fully porous particles of larger diameter (5μm), the pressure drop is also increased. Fortunately, supercritical fluids have a low viscosity, which allows coupling several columns to achieve high N values, while maintaining flow rate above 1ml/min, ensuring a ultra high efficiency (UHE) at low pressure (LP) (below 40MPa), with regards to the one reached with liquid and sub-two micron particles (around 100MPa). The use of two detector systems (UV and ELSD) connected in series to the UHE-LP-SFC system provides complementary responses, due to their specific detection principles. Working in a first part with three coupled Kinetex C18 columns (45cm total length), the effect of modifier nature and percentage were studied with two reference oils, argan and rapeseed, chosen for their different and well-known TG composition. The analytical method was developed from previous studies performed with fully porous particles (FPP). Optimized conditions with three Kinetex were as follows: 17°C, 12% of ACN/MeOH (90/10; v/v). With these conditions, and by using an increased length of Kinetex C18 column (60cm), another additional column was selected from ten different commercial SPP C18 bonded phases, by applying a Derringer function on varied parameters: theoretical plate number (TPN), separation index (SI) for critical pairs of peaks (the peaks of compounds difficult to separate due to subtle structural differences), the analysis duration, and the total peak number. This function normalizes the values of any parameters, between 0 and 1, from the worst value to the better, allowing to take account of various parameters in the final

  19. Ambient temperature nanoelectrospray ion mobility detector for high performance liquid chromatography in determining amines.

    Science.gov (United States)

    Chen, Chuang; Hou, Keyong; Wang, Weiguo; Li, Jinghua; Li, Haiyang

    2014-09-01

    A nanoelectrospray ionization ion mobility spectrometer (nanoESI-IMS) working at ambient pressure and ambient temperature was developed as a detector of high performance liquid chromatography (HPLC) to achieve sensitive detection of amines with no derivatization and meanwhile provide another dimension of separation. The easier desolvation property of the charged droplets formed in nanoESI source enabled complete desolvation of the product ions of sixteen amines and drugs using the nanoESI-IMS at ambient temperature. Working at ambient temperature was good for suppressing the dissociation of thermal volatile ions, such as only the proton adducted molecular ions were observed for morphine in the nanoESI-IMS. Besides, the resolving power of the nanoESI-IMS also showed an increasing tendency as lowering the working temperature, an increment of 19 percent and 10 percent was observed for diethylamine and triethylamine as the temperature dropped from 92°C to 32°C. The resolving power of the nanoESI-IMS at 32°C for the 16 tested compounds was amid 33-44. With the nanoESI-IMS coupled to HPLC, a six-compound mixture including isomers was successfully separated and detected without any derivatization. And linear response ranges of 1 to 20, 0.5 to 20, and 0.8 to 20μgml(-1) and limits of detection of 0.25, 0.15, and 0.17μgml(-1) for triethylamine, diethylamine, and butylamine, respectively, were obtained with the hyphenated system. These results showed the excellent performance of the two-dimensional separation and detection method in direct qualitative and quantitative analyses of amines.

  20. Trace-level determination of sweeteners in sewage sludge using selective pressurized liquid extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Arbeláez, Paula; Borrull, Francesc; Maria Marcé, Rosa; Pocurull, Eva

    2015-08-21

    The occurrence of sweeteners in the environment has become a matter of concern due to the possibility of adverse effects on human health and wildlife species. One of the routes by which sweeteners enter the environment is through sewage sludge. Therefore, a method was developed with a selective-pressurized liquid extraction (S-PLE) followed by liquid chromatography-tandem mass spectrometry for the simultaneous determination of eight sweeteners in sewage sludge. The chromatographic separation was achieved in less than ten minutes using an amide polar-embedded reversed-phase column. Due to the high matrix effect present in the sample, an extensive study was conducted in order to overcome this issue, with C18 in-cell and solid-phase extraction (Oasis HLB) as a clean-up method. S-PLE/SPE recoveries at two levels of concentration (50μg/kg and 1000μg/kg in dry weight (d.w.), n=5) were higher than 61%. Repeatability and reproducibility at the same concentrations (%RSD, n=5) were lower than 11% and 16%, respectively. The limits of detection were 10μg/kg (d.w) for all compounds, except for cyclamate (5μg/kg (d.w.)). The method was successfully applied to sewage sludge samples from three sewage treatment plants located in Catalonia (Spain). Of the eight compounds, five were determined in all of the samples analysed, with acesulfame and saccharine being recorded at the highest concentrations of up to 481μg/kg and 591μg/kg (d.w.), respectively.

  1. Determination of enantiomeric impurity of etomidate by high performance liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Objective To determine enantiomeric impurity of etomidate using high performance liquid chromatography. Methods (R)-etomidate and (S)-etomidate were separated on a CHIRALPAK AD-H column. The mobile phase consisted of 20∶80(v/v) isopropanol-n-hexane. The flow rate of the mobile phase was 0.5mL/min. The detected wavelength was 242nm. Results (R)-etomidate and (S)-etomidate could be separated completely under these conditions. The precision of (R)-etomidate was 1.57% (n=3). The limit of detection of (R)-etomid...

  2. Anomalous properties of flavonoids in reversed phase high performance liquid chromatography

    Science.gov (United States)

    Zenkevich, I. G.; Gushchina, S. V.

    2011-09-01

    It is shown through reversed phase high performance liquid chromatography that a characteristic feature of such abundant natural flavonoids as flavon-3-ols is an anomalously strong antibate dependence of their retention indices ( RI) on the organic solvent concentration ( C) in the eluent, dRI/ dC < 0. In order to interpret this anomaly, the specific optical rotation values [α]{D/20} of natural (+)-(2 R,3 R)-dihydroquercetin in different solvents are compared, confirming the reverse formation of hydrated flavonoids in aqueous solutions.

  3. Study of Saiga Horn Using High-Performance Liquid Chromatography with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Kateřina Mikulíková

    2012-01-01

    Full Text Available The saiga horns have been investigated the using of modern analytic methods. High-performance liquid chromatography (HPLC with mass-spectrometric (MS and MS/MS detection and polyacrylamide gel electrophoresis (PAGE were used. It could be concluded that basic proteins of the saiga horns are keratins and collagen. The basic representation protein in all samples is keratin type I microfibrillar (from sheep, keratin type II microfibrillar (from sheep, collagen type I (α1 (from bovine and collagen type I (α2 (from bovine. Free amino acids we determined in all samples are nontreated by enzyme.

  4. On-line radiochemical assay for monoamine oxidase utilizing high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Nissinen, E.; Linko-Loeppoenen SMae; Maennistoe P4

    1984-12-01

    A fast and sensitive assay for the determination of monoamine oxidase activity was developed. The method is based on the separation and quantitation of /sup 14/C-labeled assay products by high-performance liquid chromatography, which is interfaced directly into a flow-through radioactivity detector. This allows on-line quantitation of the radioactive compounds with picomole sensitivity. The method makes possible the complete separation and detection of the deaminated products of monoamine oxidase A and B substrates benzylamine and 5-hydroxytryptamine, respectively. This assay has been applied to the measurement of monoamine oxidase A and B activities in rat brain.

  5. Detection of cheese whey and caseinomacropeptide in fermented milk beverages using high performance liquid chromatography

    OpenAIRE

    E.H.P. Andrade; M.R. Souza; Fonseca,L.M.; C.F.A.M. Penna; M.M.O.P. Cerqueira; T. Roza; Seridan,B.; M.F.S. Resende; Pinto, F. A.; C.N.B.C. Villanoeva; Leite,M.O.

    2014-01-01

    Cheese whey level and caseinomacropeptide (CMP) index of fermented milk beverages added with four levels of cheese whey (0, 10, 20, and 40%) and stored at 8-10oC for 0, 7, 14 and 21 days were determined by high performance liquid chromatography-gel filtration (HPLC-GF). Additionally, the interference of the starter culture and the storage time on the detection of cheese whey and CMP were investigated. Refrigerated storage up to 21 days did not affect (P>0.05) cheese whey and CMP amounts in mi...

  6. Determination of rhoifolin and daidzin in human plasma by high-performance liquid chromatography.

    Science.gov (United States)

    Ishii, K; Urano, S; Furuta, T; Kasuya, Y

    1994-05-13

    A method for determining flavonoids in human plasma is presented for application to pharmacokinetic studies of two flavonoids, rhoifolin and daidzin. Isocratic reversed-phase high-performance liquid chromatography (HPLC) was used with genistin as an internal standard and solid-phase extraction using a Sep-Pak C18 cartridge. The mobile phases were acetonitrile-0.1 M ammonium acetate solution (20:80, v/v) for rhoifolin and methanol-0.1 M ammonium acetate solution (33:67, v/v) for daidzin. The detection limits on-column were 2 ng for rhoifolin and 0.5 ng for daidzin.

  7. Separation of polyamines, conjugated to DNA, by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Mateos, J L; Reyes, A; Vicente, C; Legaz, M E

    2000-02-18

    Genomic DNA was isolated from the lichen Evernia prunastri in order to analyze by high-performance liquid chromatography the occurrence of polyamines conjugated to the macromolecule. The acid-insoluble (PH) fraction of this DNA contained mainly conjugated spermidine, although small amounts of free putrescine and spermidine were also present. The PH fraction of DNA also contained conjugated evernic acid, the main phenol produced by this lichen species. Conjugation of polyamines to calf thymus DNA was carried out under in vitro conditions. Conjugation was to spermidine and mainly to spermine and produced DNA compactation. Evernic acid enhanced the action of polyamines in order to produce DNA aggregation.

  8. Determination of fenbendazole, praziquantel and pyrantel pamoate in dog plasma by high-performance liquid chromatography.

    Science.gov (United States)

    Morovján, G; Csokán, P; Makranszki, L; Abdellah-Nagy, E A; Tóth, K

    1998-02-27

    Simple and rapid high-performance liquid chromatographic methods were developed for the determination of fenbendazole, praziquantel and pyrantel pamoate in dog plasma. The combination of these drugs is the most powerful treatment against most types of worms. Blood plasma samples obtained in a pharmacokinetic trial were prepared using solid-phase extraction. Fenbendazole and praziquantel were analyzed simultaneously by reversed-phase high-performance liquid chromatography on an octadecyl-modified silica stationary phase employing acetonitrile-phosphate buffer (pH 3.0) eluent and ultraviolet detection at 220 nm. Pyrantel was analyzed separately on a base-deactivated reversed-phase column using methanol-tetrahydrofuran-ammonium acetate buffer (pH 4.6) eluent and ultraviolet detection at 317 nm. Average recoveries for fenbendazole, praziquantel and pyrantel pamoate were 76.8, 93.4 and 90.5%, respectively. Limits of quantitation were in the range of 15-25 ng/ml plasma.

  9. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses.

    Science.gov (United States)

    Muthukrishnan, Suriyavathana; Palanisamy, Subha; Subramanian, Senthilkumar; Selvaraj, Sumathi; Mari, Kavitha Rani; Kuppulingam, Ramalingam

    2016-08-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy) tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases.

  10. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    Directory of Open Access Journals (Sweden)

    Suriyavathana Muthukrishnan

    2016-08-01

    Full Text Available Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV were identified by using high-performance liquid chromatography (HPLC and gas chromatography-mass spectroscopy (GC-MS analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases.

  11. 全自动加压溶剂萃取——高效液相色谱法测定洋葱中芦丁和槲皮素含量%Determination of Contents of Rutin and Quercetin in Onion by Automated Pressurized Liquid Extractor and High Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    刘新艳; 张延国; 邹积鑫; 徐东辉; 李凌云; 刘肃

    2011-01-01

    通过与水浴回流法比较,建立了全自动加压溶剂萃取法,可简单、快速测定洋葱中保健活性物质芦丁和槲皮素含量.采用高效液相色谱仪在368nm波长处测定芦丁和槲皮素含量.色谱柱为C18柱,流动相为甲醇-磷酸溶液(58:42,体积比),以1.0ml/min流速等度洗脱,外标法定量.结果表明,在芦丁和槲皮素质量浓度为0.1~200mg/L时,其线性相关系数均大于0.999.在2.0~100mg/kg的添加水平下,芦丁和槲皮素的平均回收率分别为83.5%~94_2%和84.8%~91.2%;相对标准偏差分别为2.9%~7.4%和4.2%~6.9%(n=6).全自动加压溶剂萃取法的检出限(LOD),芦丁和槲皮素分别为0.05,0.03mg/kg.定量限(LOQ),芦丁和槲皮素分别为0.2,0.1mg/kg.研究建立的运用全自动加压溶剂萃取仪提取、高效液相色谱测定洋葱中芦丁和槲皮素的方法,线性良好,重现性较好,灵敏度较高,能够满足蔬菜和水果等农产品中芦丁和槲皮素的快速检测.%As compared with the water circumfluence method, a simple and rapid method was developed for the determination of contents of rutin and quercetin in onion by Automated Pressurized Liquid Extractor (APLE).The contents of rutin and quercetin were first determined by High Performance Liquid Chromatography (HPLC) in 368nm and analyzed on the C18 column by a isocratic elution,using a mixture of methanol~phosphoric acid solution (58:42, V/V) as the mobile phase with a flow rate of 1.0mL/min.The method is calibrated by an external standard method.Under the optimal conditions, the correlation coefficient of rutin and quercetin in the concentration range of 0.1~200mg/L is more than 0.999.The average recovery rates of rutin and quercetin in the spiked range of 2.0~100mg/kg are 83.5%~94.2% and 84.8%~91.2%, respectively.And the relative standard deviations are 2.9%~7.4% and 4.2%~6.9%,respectively (n=6).Using the automated pressurized liquid extractor method, the

  12. Determination of Aspartame, Caffeine, Saccharin, and Benzoic Acid in Beverages by High Performance Liquid Chromatography.

    Science.gov (United States)

    Delaney, Michael F.; And Others

    1985-01-01

    Describes a simple and reliable new quantitative analysis experiment using liquid chromatography for the determinaiton of caffeine, saccharin, and sodium benzoate in beverages. Background information, procedures used, and typical results obtained are provided. (JN)

  13. Characterization of the chemical composition of a block copolymer by liquid chromatography/mass spectrometry using atmospheric pressure chemical ionization and electrospray ionization

    NARCIS (Netherlands)

    Leeuwen, van Suze M.; Tan, BoonHua; Grijpma, Dirk W.; Feijen, J.; Karst, Uwe

    2007-01-01

    Liquid chromatography/mass spectrometry (LC/MS) with electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) in the positive and negative ion modes was used for the characterization of a block copolymer consisting of methoxy poly(ethylene oxide) (mPEO), an -caprolactone (CL

  14. Characterization of the chemical composition of a block copolymer by liquid chromatography/mass spectrometry using atmospheric pressure chemical ionization and electrospray ionization

    NARCIS (Netherlands)

    van Leeuwen, Suze M.; Tan, BoonHua; Grijpma, Dirk W.; Fejen, Jan; Karst, Uwe

    2007-01-01

    Liquid chromatography/mass spectrometry (LC/MS) with electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) in the positive and negative ion modes was used for the characterization of a block copolymer consisting of methoxy poly(ethylene oxide) (mPEO), an epsilon-caprolact

  15. Simultaneous determination of airborne carbamates in workplace by high performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Li, Hong-Ping; Li, Jen-Hou; Li, Gwo-Chen; Jen, Jen-Fon

    2004-06-17

    A high performance liquid chromatography with fluorescence (HPLC-F) detector was examined to simultaneous determination of airborne carbamates in the workplace of manufactory. The OVS-2 air sampling tube filled with glass fiber filter or quartz fiber and combined filter/XAD-2 were evaluated to collect nine commonly used carbamates (Carbofuran, Isoprocarb, Methomyl, Metolcarb, Thiodicarb, Carbaryl, Oxamyl, Methiocarb, and Prpoxur) from the air of manufactory in high humidity country. After being extracted with acetonitrile from sampling tubes, the carbamates were determined by high performance liquid chromatography with fluorescence detection posterior to on-line derivatization. The collection of carbamates and the recovery of extraction from glass wool fiber in several concentration levels, and from quartz filter were evaluated. The storage stability of carbamates was also tested. Results indicated that the HPLC-fluorescence method offers satisfactory resolution and sensitivity in carbamate analysis. With the glass fiber filter and combined filter/XAD-2, the Carbofuran, Isoprocarb, Methomyl, Metolcarb, and Thiodicarb were stable for a 28-day storage test, Carbaryl and Oxamyl for 14 days, and Methiocarb and Prpoxur for 7 days. All of these pesticides were with detection limit of 3mugm(-3). It is suited for environmental monitoring. The airborne carbamates in different areas of the manufactory were measured.

  16. Saffron authentication based on liquid chromatography high resolution tandem mass spectrometry and multivariate data analysis.

    Science.gov (United States)

    Rubert, Josep; Lacina, Ondrej; Zachariasova, Milena; Hajslova, Jana

    2016-08-01

    Saffron is one of the oldest and most expensive spices, which is often target of fraudulent activities. In this research, a new strategy of saffron authentication based on metabolic fingerprinting was developed. In the first phase, a solid liquid extraction procedure was optimized, the main aim was to isolate as maximal representation of small molecules contained in saffron as possible. In the second step, a detection method based on liquid chromatography coupled with high-resolution mass spectrometry was developed. Initially, principal component analysis (PCA) revealed clear differences between saffron cultivated and packaged in Spain, protected designation of origin (PDO), and saffron packaged in Spain of unknown origin, labeled Spanish saffron. Afterwards, orthogonal partial least square discriminant analysis (OPLS-DA) was favorably used to discriminate between Spanish saffron. The tentative identification of markers showed glycerophospholipids and their oxidized lipids were significant markers according to their origin.

  17. Extraction and determination of hormones in cosmetics by homogeneous ionic liquid microextraction high-performance liquid chromatography.

    Science.gov (United States)

    Kang, Mingqin; Sun, Shuo; Li, Na; Zhang, Daihui; Chen, Mingyan; Zhang, Hanqi

    2012-08-01

    The homogeneous ionic liquid microextraction was applied to the extraction of hormones from cosmetics and the hormones were determined by high-performance liquid chromatography. 1-Hexyl-3-methylimidazolium tetrafluoroborate was used as extraction solvent. Ammonium hexafluorophosphate as used as ion-pairing agent. Several experimental parameters, including the volume of 1-hexyl-3-methylimidazolium tetrafluoroborate, amount of ammonium hexafluorophosphate and sodium chloride, extraction and centrifuge time, and the pH value, were optimized. The limits of detection and quantification for the analytes ranged from 0.03 to 0.24 ng/mL and from 0.10 to 0.79 ng/mL, respectively. The precision for determining the hormones was lower than 5.2%. The proposed method was successfully developed for the determination of hormones in real cosmetic samples.

  18. Determination of Four Pesticides in Soil by Homogeneous Ionic Liquid-based Microextraction Coupled with High-performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    YAN Rui; SHAO Ming-yuan; LIANG Zhen-fen; ZHANG Han-qi; YU Ai-min

    2013-01-01

    Homogeneous ionic liquid microextraction was developed for the simultaneceus extraction of dimethomorph,mefenacet,isoprothiolane and oxadiazon from soil.1-Butyl-3-methylimidazolium tetrafluoroborate was used as extraction solvent,and ammonium hexafluorophosphate was used as ion-pairing agent.High-performance liquid chromatography(HPLC) was employed for separation and determination of the analytes.The calibration curves show good linear relationship(r>0.9988).The recoveries are between 74.2% and 97.9% with relative standard deviations(RSDs) lower than 5.97%.The present method is free of volatile organic solvents,and expenditures of sample,extraction time and solvent are lower,compared with ultrasonic and Soxhlet extraction.There was no obvious difference in the extraction recoveries of pesticides obtained by the three extraction methods.

  19. Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

    2015-06-01

    An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography.

  20. Structural analysis of liquid aluminum at high pressure and high temperature using the hard sphere model

    Science.gov (United States)

    Ikuta, Daijo; Kono, Yoshio; Shen, Guoyin

    2016-10-01

    The structure of liquid aluminum is measured up to 6.9 GPa and 1773 K using a multi-angle energy-dispersive X-ray diffraction method in a Paris-Edinburgh press. The effect of pressure and temperature on the structure and density of liquid aluminum is analyzed by means of the hard sphere model. Peak positions in the structure factor of liquid aluminum show a nearly constant value with varying temperatures at ˜1-2 GPa and slightly change with varying pressures up to 6.9 GPa at 1173-1773 K. In contrast, the height of the first peak in the structure factor significantly changes with varying pressures and temperatures. Hard sphere model analysis shows that the structure of liquid aluminum in the pressure-temperature range of this study is controlled mostly by the packing fraction with only a minor change in hard sphere diameters. The obtained packing fractions and hard sphere diameters are used to calculate densities of liquid aluminum at high pressure-temperature conditions.

  1. Pressurized liquid extraction-gas chromatography-mass spectrometry analysis of fragrance allergens, musks, phthalates and preservatives in baby wipes.

    Science.gov (United States)

    Celeiro, Maria; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria

    2015-03-01

    Baby wipes and wet toilet paper are specific hygiene care daily products used on newborn and children skin. These products may contain complexes mixtures of harmful chemicals. A method based on pressurized liquid extraction (PLE) followed by gas chromatography-mass spectrometry (GC-MS) has been developed for the simultaneous determination of sixty-five chemical compounds (fragrance allergens, preservatives, musks, and phthalates) in wipes and wet toilet paper for children. These compounds are legislated in Europe according Regulation EC No 1223/2009, being twelve of them banned for their use in cosmetics, and one of them, 3-iodo-2-propynyl butylcarbamate (IPBC), is banned in products intended for children under 3 years. Also, propyl-, and butylparaben will be prohibited in leave-on cosmetic products designed for application on the nappy area of children under 3 years from April 2015. PLE is a fast, simple, easily automated technique, which permits to integrate a clean-up step during the extraction process reducing analysis time and stages. The proposed PLE-based procedure was optimized on real non-spiked baby wipe samples by means of experimental design to study the influence on extraction of parameters such as extraction solvent, temperature, extraction time, and sorbent type. Under the selected conditions, the method was validated showing satisfactory linearity, and intra-day, and inter-day precision. Recoveries were between 80-115% for most of the compounds with relative standard deviations (RSD) lower than 15%. Finally, twenty real samples were analyzed. Thirty-six of the target analytes were detected, highlighting the presence of phenoxyethanol in all analyzed samples at high concentration levels (up to 0.8%, 800μgg(-1)). Methyl paraben (MeP), and ethyl paraben (EtP) were found in 40-50% of the samples, and the recently banned isobutyl paraben (iBuP) and isopropyl paraben (iPrP), were detected in one and seven samples, respectively, at concentrations between

  2. Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

    Science.gov (United States)

    Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

    2015-07-01

    Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns.

  3. Hb A1c Separation by High Performance Liquid Chromatography in Hemoglobinopathies

    Science.gov (United States)

    Chandrashekar, Vani

    2016-01-01

    Hb A1c measurement is subject to interference by hemoglobin traits and this is dependent on the method used for determination. In this paper we studied the difference between Hb A1c measured by HPLC in hemoglobin traits and normal chromatograms. We also studied the correlation of Hb A1c with age. Hemoglobin analysis was carried out by high performance liquid chromatography. Spearman's rank correlation was used to study correlation between A1c levels and age. Mann-Whitney U test was used to study the difference in Hb A1c between patients with normal hemoglobin and hemoglobin traits. A total of 431 patients were studied. There was positive correlation with age in patients with normal chromatograms only. No correlation was seen in Hb E trait or beta thalassemia trait. No significant difference in Hb A1c of patients with normal chromatograms and patients with hemoglobin traits was seen. There is no interference by abnormal hemoglobin in the detection of A1c by high performance liquid chromatography. This method cannot be used for detection of A1c in compound heterozygous and homozygous disorders. PMID:26989559

  4. Hb A1c Separation by High Performance Liquid Chromatography in Hemoglobinopathies

    Directory of Open Access Journals (Sweden)

    Vani Chandrashekar

    2016-01-01

    Full Text Available Hb A1c measurement is subject to interference by hemoglobin traits and this is dependent on the method used for determination. In this paper we studied the difference between Hb A1c measured by HPLC in hemoglobin traits and normal chromatograms. We also studied the correlation of Hb A1c with age. Hemoglobin analysis was carried out by high performance liquid chromatography. Spearman’s rank correlation was used to study correlation between A1c levels and age. Mann-Whitney U test was used to study the difference in Hb A1c between patients with normal hemoglobin and hemoglobin traits. A total of 431 patients were studied. There was positive correlation with age in patients with normal chromatograms only. No correlation was seen in Hb E trait or beta thalassemia trait. No significant difference in Hb A1c of patients with normal chromatograms and patients with hemoglobin traits was seen. There is no interference by abnormal hemoglobin in the detection of A1c by high performance liquid chromatography. This method cannot be used for detection of A1c in compound heterozygous and homozygous disorders.

  5. Determination of furanochromones and pyranocoumarins in drugs and Ammi visnaga fruits by combined solid-phase extraction-high-performance liquid chromatography and thin-layer chromatography-high-performance liquid chromatography.

    Science.gov (United States)

    Zgórka, G; Dragan, T; Głowniak, K; Basiura, E

    1998-02-27

    A new, simple and rapid solid-phase extraction method for the determination of furanochromones and pyranocoumarins in Ammi visnaga L. fruits and pharmaceuticals by reversed-phase high-performance liquid chromatography (RP-HPLC) was developed. The isolation of compounds examined was carried out on octadecyl BakerBond SPE columns using various concentrations of methanol, acetonitrile and tetrahydrofuran in water. High and reproducible recoveries were obtained. To compare the results of quantitative analysis a preparative TLC procedure was also elaborated and carried out.

  6. New ultrasonic Bleustein-Gulyaev wave method for measuring the viscosity of liquids at high pressure

    Science.gov (United States)

    Kiełczyński, P.; Szalewski, M.; Siegoczyński, R. M.; Rostocki, A. J.

    2008-02-01

    In this paper, a new method for measuring the viscosity of liquids at high pressure is presented. To this end the authors have applied an ultrasonic method using the Bleustein-Gulyaev (BG) surface acoustic wave. By applying the perturbation method, we can prove that the change in the complex propagation constant of the BG wave produced by the layer of liquid loading the waveguide surface is proportional to the shear mechanical impedance of the liquid. In the article, a measuring setup employing the BG wave for the purpose of measuring the viscosity of liquids at high pressure (up to 1GPa) is presented. The results of high-pressure viscosity measurements of triolein and castor oil are also presented. In this paper the model of a Newtonian liquid was applied. Using this new method it is also possible to measure the viscosity of liquids during the phase transition and during the decompression process (hysteresis of the dependence of viscosity on pressure).

  7. Pressurized liquid extraction followed by gas chromatography with atomic emission detection for the determination of fenbutatin oxide in soil samples.

    Science.gov (United States)

    Canosa, P; Montes, R; Lamas, J P; García-López, M; Orriols, I; Rodríguez, I

    2009-08-15

    A novel method for the determination of the miticide bis[tris(2-methyl-2-phenylpropyl)tin] oxide, also known as fenbutatin oxide (FBTO), in agricultural soils is presented. Pressurized liquid extraction (PLE) followed by analyte derivatization and extraction into isooctane was the used sample preparation approach. Selective determination was achieved by gas chromatography with atomic emission detection (GC-AED). Influence of different parameters on the performance of the extraction process is thoroughly discussed; moreover, some relevant aspects related to derivatization, determination and quantification steps are also presented. As regards PLE, the type of solvent and the temperature were the most relevant variables. Under optimized conditions, acetone, without any acidic modifier, was employed as extractant at 80 degrees C. Cells were pressurized at 1500 psi, and 2 static cycles of 1 min each were applied. Acetone extracts (ca. 25 mL) were concentrated to 1 mL, derivatized with sodium tetraethyl borate (NaBEt(4)) and the FBTO derivative, resulting from cleavage of the Sn-O-Sn bond followed by ethylation of the hydroxyl fragments, extracted into isooctane and determined by GC-AED. Under final working conditions, the proposed method provided recoveries from 76 to 99% for spiked soil samples, a limit of quantification of 2 ng g(-1) and an acceptable precision. Analysis of samples from vineyards sprayed with FBTO, confirmed the persistence of the miticide in soil for more than 1 year after being applied.

  8. Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

    2015-09-01

    In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples.

  9. Ultrasound-assisted dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-fluorescence detection for sensitive determination of biogenic amines in rice wine samples.

    Science.gov (United States)

    Huang, Ke-Jing; Wei, Cai-Yun; Liu, Wei-Li; Xie, Wan-Zhen; Zhang, Jun-Feng; Wang, Wei

    2009-09-18

    Ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography-fluorescence detection was used for the extraction and determination of three biogenic amines including octopamine, tyramine and phenethylamine in rice wine samples. Fluorescence probe 2,6-dimethyl-4-quinolinecarboxylic acid N-hydroxysuccinimide ester was applied for derivatization of biogenic amines. Acetonitrile and 1-octanol were used as disperser solvent and extraction solvent, respectively. Extraction conditions including the type of extraction solvent, the volume of extraction solvent, ultrasonication time and centrifuging time were optimized. After extraction and centrifuging, analyte was injected rapidly into high-performance liquid chromatography and then detected with fluorescence. The calibration graph of the proposed method was linear in the range of 5-500 microg mL(-1) (octopamine and tyramine) and 0.025-2.5 microg mL(-1) (phenethylamine). The relative standard deviations were 2.4-3.2% (n=6) and the limits of detection were in the range of 0.02-5 ng mL(-1). The method was applied to analyze the rice wine samples and spiked recoveries in the range of 95.42-104.56% were obtained. The results showed that ultrasound-assisted dispersive liquid-liquid microextraction was a very simple, rapid, sensitive and efficient analytical method for the determination of trace amount of biogenic amines.

  10. Validation of a technique by high-performance liquid chromatography for the determination of total isoflavones

    Directory of Open Access Journals (Sweden)

    Pilar A. Soledispa Cañarte

    2017-04-01

    Full Text Available Context: Isoflavones may act as selective regulators in the prevention of various diseases. The most important source of isoflavones is the soy, from which different phytotherapeutics are elaborated of use in Ecuadorian population. However, its concentration varies depending on several factors, therefore quality assessment need to be carried out through out several analytical methods. Aims: To validate an analytical method by high precision liquid chromatography (HPLC to quantify total isoflavones in herbal medicine. Methods: To quantify isoflavones, it was used a brand liquid chromatography with UV/VIS detector at 260 nm, C-18 column using isocratic method. The mobile phase was composed of 2% acetic acid: acetonitrile (75:25. The quantification was performed against reference standard. The parameters for the validation followed the established in the USP 33. Results: The chromatogram presented six peaks with elution between 1.557 and 18.913 min. The linearity of the system and the method got r2 equal to 0.98 and 0.99 respectively. The coefficients of variation 1.5% in the study of repetitiveness and 2% in intermediate precision. The accuracy of the adjusted lineal model exhibited r=0.95 and intercept reliable interval (-0.921; 1.743. Conclusions: The validated method was specific, accurate, precise and linear. It can be used for quality control and stability studies of isoflavones present in herbal medicine.

  11. Development of high performance liquid chromatography method for miconazole analysis in powder sample

    Science.gov (United States)

    Hermawan, D.; Suwandri; Sulaeman, U.; Istiqomah, A.; Aboul-Enein, H. Y.

    2017-02-01

    A simple high performance liquid chromatography (HPLC) method has been developed in this study for the analysis of miconazole, an antifungal drug, in powder sample. The optimized HPLC system using C8 column was achieved using mobile phase composition containing methanol:water (85:15, v/v), a flow rate of 0.8 mL/min, and UV detection at 220 nm. The calibration graph was linear in the range from 10 to 50 mg/L with r 2 of 0.9983. The limit of detection (LOD) and limit of quantitation (LOQ) obtained were 2.24 mg/L and 7.47 mg/L, respectively. The present HPLC method is applicable for the determination of miconazole in the powder sample with a recovery of 101.28 % (RSD = 0.96%, n = 3). The developed HPLC method provides short analysis time, high reproducibility and high sensitivity.

  12. Quantitative determination of gibberellins by high performance liquid chromatography from various gibberellins producing Fusarium strains.

    Science.gov (United States)

    Bhalla, Kirti; Singh, Shashi Bala; Agarwal, Rashmi

    2010-08-01

    High performance liquid chromatographic (HPLC) method was developed for analysis of seven gibberellins, i.e., GA3, GA4, GA7, GA3 methyl ester, GA7 methyl ester 3,13 diacetate, GA7 methyl ester, and fusaric acid, using an isocratic system. Method was used for estimation of gibberellins from different Fusarium strains. Gibberellins were extracted from 28 strains of Fusarium, out of which six strains of Fusarium were isolated from soil of different parts of India and 22 strains were procured from the Indian Type Culture Collection, Indian Agricultural Research Institute, New Delhi. Extracts were analyzed for qualitative and quantitative estimation of gibberellins by thin layer chromatography and HPLC, respectively. On the basis of quantitative analysis of produced gibberellins by HPLC, they were categorized as low, moderate, and high gibberellin producing strain. For the first time, Fusarium solani was also reported as high GA3 producing strain.

  13. Discussions about high performance liquid chromatography upgrading to ion chromatography%液相色谱升级改造为离子色谱问题探讨

    Institute of Scientific and Technical Information of China (English)

    施超欧; 马浩; 姚宝龙; 黄彩勇

    2014-01-01

    离子色谱作为色谱的一个分支,在原理和仪器结构上与液相色谱密切相关。本文总结了液相色谱升级为离子改造色谱的经验。%As a part of chromatography ,the functions and structures of instruments between high per-formance liquid chromatography and ion chromatography are closely related .In this paper ,HPLC upgra-ded to IC was discused .

  14. Ionic liquids for improving the extraction of NSAIDs in water samples using dispersive liquid-liquid microextraction by high performance liquid chromatography-diode array-fluorescence detection.

    Science.gov (United States)

    Toledo-Neira, Carla; Álvarez-Lueje, Alejandro

    2015-03-01

    A rapid, sensitive and efficient analytical method based on the use of ionic liquids for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed. High-performance liquid chromatography equipped with a diode array and fluorescence detector was used for quantification of ketoprofen, ibuprofen and diclofenac in tap and river water samples. This new method relies on the use of two ionic liquids with multiple functionalities: one functions as an extraction solvent (1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF6]), and the other changes the polarity in the aqueous medium (1-butyl-3-methylimidazolium tetrafluoroborate, ([BMIM][BF4]). Factors such as the type and volume of the ILs and dispersive solvent, sample volume, and centrifugation time were investigated and optimized. The optimized method exhibited good precision, with relative standard deviation values between 2% and 3%, for the three NSAIDs. Limits of detection achieved for all of the analytes were between 17 and 95 ng mL(-1), and the recoveries ranged from 89% to 103%. Furthermore, the enrichment factors ranged from 49 to 57. The proposed method was successfully applied to the analysis of NSAIDs in tap and river water samples.

  15. Highly efficient peptide separations in proteomics Part 1. Unidimensional high performance liquid chromatography.

    Science.gov (United States)

    Sandra, Koen; Moshir, Mahan; D'hondt, Filip; Verleysen, Katleen; Kas, Koen; Sandra, Pat

    2008-04-15

    Sample complexity and dynamic range constitute enormous challenges in proteome analysis. The back-end technology in typical proteomics platforms, namely mass spectrometry (MS), can only tolerate a certain complexity, has a limited dynamic range per spectrum and is very sensitive towards ion suppression. Therefore, component overlap has to be minimized for successful mass spectrometric analysis and subsequent protein identification and quantification. The present review describes the advances that have been made in liquid-based separation techniques with focus on the recent developments to boost the resolving power. The review is divided in two parts; the first part deals with unidimensional liquid chromatography and the second part with bi- and multidimensional liquid-based separation techniques. Part 1 mainly focuses on reversed-phase HPLC due to the fact that it is and will, in the near future, remain the technique of choice to be hyphenated with MS. The impact of increasing the column length, decreasing the particle diameter, replacing the traditional packed beds by monolithics, amongst others, is described. The review is complemented with data obtained in the laboratories of the authors.

  16. Quantification of achiral and chiral methylsulfonyl polychlorinated biphenyl metabolites by column-switching liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry.

    Science.gov (United States)

    Cooper, Victoria I; Letcher, Robert J; Dietz, Rune; Sonne, Christian; Wong, Charles S

    2012-12-14

    An enantioselective heart-cut column-switching liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry method was developed for the analysis of 25 methylsulfonyl polychlorinated biphenyl metabolites in tissue extracts. Use of a pyrenyl-ethyl silica column in the first dimension enabled separation of all but two pairs of isobaric analytes. Enantioseparation was achieved for 9 out of the 10 atropisomeric analytes using a Chiralpak AD-H amylose-based column within 93 min, resulting in greater chromatographic resolution of enantioseparation over shorter analysis time by up to a factor of three, compared to previous one-dimensional and multi-dimensional gas chromatography-based methods. Precision for concentration and enantiomer fraction measurements was within 11% and 3% relative standard deviation, respectively. Limits of detection ranged from 0.01 to 1.73 ng on-column. Meta-congeners had poorer sensitivity (i.e., ng on-column), consistent with existing gas chromatography-based methods. Despite this limitation, the method was successfully applied to the analysis of Greenland sledge dog adipose tissue extracts, which had highly non-racemic residues of 4-methylsulfonyl-2,2',3,5',6-pentachlorobiphenyl and 4'-methylsulfonyl-2,2',3,3',4,6'-hexachlorobiphenyl, consistent with past reports in Arctic mammals.

  17. Design and implementation of an automated liquid-phase microextraction-chip system coupled on-line with high performance liquid chromatography

    DEFF Research Database (Denmark)

    Li, Bin; Petersen, Nickolaj J.; Payán, María D Ramos

    2014-01-01

    An automated liquid-phase microextraction (LPME) device in a chip format has been developed and coupled directly to high performance liquid chromatography (HPLC). A 10-port 2-position switching valve was used to hyphenate the LPME-chip with the HPLC autosampler, and to collect the extracted...

  18. High pressure dewatering of liquid manure; Hoejtryksafvanding af gylle

    Energy Technology Data Exchange (ETDEWEB)

    Koch, T.

    1999-08-01

    The purpose of this work is to develop a dewatering method that can dewater digested manure to a dry matter content that makes it possible to utilise the dry matter for energy production. Many tests of existing analysis methods for liquid manure. None of the mathods have shown any acceptable correlation's between the results and obtained dewatering characteristics. This project have not developed any analysis methods that can predict the mechanical behaviour of manure. But the dewatering device that has been developed works, and can dewater manure. It has been proved that it is possible to dewater digested manure up to 59-60% dry matter content in laboratory conditions. (dewatering time 10-20 minutes and a pressure of up to 61 MPa). The experiment has shown that the maximum obtainable pressure in the manure (before it escapes the dewatering chamber) is dependent of the speed of pressure increase. At more 'commercial' conditions (a total dewatering cycle time of 30-60 seconds) it is possible to obtain a dry matter content of 50-54%. Some times it is possible to obtain 58% dry matter content and 2 days later it is only possible to obtain 51% drymatter content. 2-10% of the ammonium and potassium and 20-40% of the phosphorous is found in the dry fraction. Fresh manure have been dewatered and the maximum obtainable dry matter content is approx. 25-35% at 5-15 MPa. In the second phase of the project it was decided to include an experiment of dewatering wet straw and straw coke. A technical note on this experiment is included as an appendix. (LN)

  19. Determination of nitrofuran metabolites in shrimp by high performance liquid chromatography with fluorescence detection and liquid chromatography-tandem mass spectrometry using a new derivatization reagent.

    Science.gov (United States)

    Du, Na-Na; Chen, Ming-Ming; Sheng, Liang-Quan; Chen, Shui-Sheng; Xu, Hua-Jie; Liu, Zhao-Di; Song, Chong-Fu; Qiao, Rui

    2014-01-31

    A high performance liquid chromatography with fluorescence detection (HPLC-FLD) method for the simultaneous determination of total nitrofuran metabolite residues (furazolidone, furaltadone, nitrofurantoin, and nitrofurazone) in shrimp was developed. The method involves the acid hydrolysis of protein-bound metabolites, followed by the derivatization of the freed metabolites with the new fluorescent derivatization reagent 2-hydroxy-1-naphthaldehyde (HN) and subsequent liquid-liquid extraction (LLE). Separation is achieved on a YMC-Pack Polymer C18 column under alkaline conditions, and the high fluorescence intensity of the derivatives at an emission wavelength Em=463nm (Ex=395nm) enables, for the first time, their simultaneous determination in shrimp at concentrations as low as 1μg/kg by HPLC-FLD. The method was validated using blank shrimp fortified with all four metabolites at 0.5, 1.0 and 2.0μg/kg. Recoveries were >87% with relative standard deviations of HPLC-FLD were in very good agreement with those obtained by LC-MS/MS analysis.

  20. Rapid determination of alpha tocopherol in olive oil adulterated with sunflower oil by reversed phase high-performance liquid chromatography.

    Science.gov (United States)

    Bakre, S M; Gadmale, D K; Toche, R B; Gaikwad, V B

    2015-05-01

    A new method is developed to determine the presence of sunflower oil in olive oil. α-tocopherol is selected as discriminating parameter for detecting sunflower oil adulterant in olive oil. Admixtures of olive oil and sunflower oil (5 %, 10 %, 15 % and 20 % sunflower oil in olive oil) are prepared. These admixtures are analysed by reversed phase high pressure liquid chromatography coupled with fluorescence detector. The sample preparation does not require saponification or addition of antioxidant. The chromatographic system consists of a C18 column with methanol: acetonitrile (50:50) mobile phase. Fluorescence detector excitation wavelength is set at 290 nm and emission wavelength is set at 330 nm. The α tocopherol concentration increases linearly in olive oil adulterated with sunflower oil. The method is simple, selective, sensitive and is precise (RSD = 2.65 %) for α tocopherol. The present method can precisely detect 5 % sunflower oil in olive oil.

  1. Methacrylate-bonded covalent-organic framework monolithic columns for high performance liquid chromatography.

    Science.gov (United States)

    Liu, Li-Hua; Yang, Cheng-Xiong; Yan, Xiu-Ping

    2017-01-06

    Covalent-organic frameworks (COFs) are a newfangled class of intriguing microporous materials. Considering their unique properties, COFs should be promising as packing materials for high performance liquid chromatography (HPLC). However, the irregular shape and sub-micrometer size of COFs synthesized via the traditional methods render the main obstacles for the application of COFs in HPLC. Herein, we report the preparation of methacrylate-bonded COF monolithic columns for HPLC to overcome the above obstacles. The prepared COF bonded monolithic columns not only show good homogeneity and permeability, but also give high column efficiency, good resolution and precision for HPLC separation of small molecules including polycyclic aromatic hydrocarbons, phenols, anilines, nonsteroidal anti-inflammatory drugs and benzothiophenes. Compared with the bare polymer monolithic column, the COF bonded monolithic columns show enhanced hydrophobic, π-π and hydrogen bond interactions in reverse phase HPLC. The results reveal the great potential of COF bonded monoliths for HPLC and COFs in separation sciences.

  2. Screening anti-tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry.

    Science.gov (United States)

    Zhang, Tao; Ding, Yuanyuan; An, Hongli; Feng, Liuxin; Wang, Sicen

    2015-07-14

    Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine-HEK293 cells were used as cell membrane stationary phase. Specificity and reproducibility of the cell membrane chromatography was evaluated using 1-tert-butyl-3-{2-[4-(diethylamino)butylamino]-6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-7-yl}urea, Nimodipine and dexamethasone acetate. Then, anti-tumor components acting on Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high-performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide-formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose-dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two-dimensional high-performance liquid chromatography method can screen and identify potential anti-tumor ingredients which specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4. This article is protected by copyright. All rights reserved.

  3. Separation of maleic anhydride grafted polypropylene using multidimensional high-temperature liquid chromatography.

    Science.gov (United States)

    Prabhu, K N; Macko, T; Brüll, R; Remerie, K; Tacx, J; Garg, P; Ginzburg, A

    2016-04-01

    Functionalization addresses a property gap of polyolefins and opens new perspectives due to improved surface properties in applications like composites (e.g., glass fiber reinforced polypropylene) and anti-corrosive coatings for metals. Various techniques have been developed to characterize functionalized polyolefins, yet no analytical approach addressing their chemical heterogeneity exists. Using High Temperature Size Exclusion Chromatography (HT-SEC) coupled to infrared spectroscopy we could show for two model samples of polypropylene grafted maleic anhydride (PP-g-MA), differing in their nominal MA content, that the grafting density increases with decreasing molar mass. Crystallization Analysis Fractionation (CRYSTAF) does not enable to separate these samples according to their composition to the extent required. Yet, when using High Temperature High Performance Liquid Chromatography (HT-HPLC), with either silica gel or Mica as stationary phase and a gradient mobile phase, a deformulation into a grafted and a non-grafted fraction could be achieved. This was confirmed by analyzing the eluted fractions by infrared spectroscopy. Hyphenating the separation according to composition with a separation according to molar mass (HT-HPLC x HT-SEC) enabled for the first time to reveal the bivariate distribution of PP-g-MA with regard to the molar mass and composition. Using on-line infrared detection quantitative information on the compositional and molar mass parameters of the individual fractions could be obtained.

  4. Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

    2016-03-04

    Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples.

  5. Ultrapreconcentration and determination of organophosphorus pesticides in water by solid-phase extraction combined with dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Chen, Junhua; Zhou, Guangming; Deng, Yongli; Cheng, Hongmei; Shen, Jie; Gao, Yi; Peng, Guilong

    2016-01-01

    Solid-phase extraction coupled with dispersive liquid-liquid microextraction was developed as an ultra-preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion-methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid-phase extraction coupled with dispersive liquid-liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid-phase extraction coupled with dispersive liquid-liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9-6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples.

  6. Determination of Harmine and Harmaline in Peganum harmala Seeds by High-Performance Liquid Chromatography

    Science.gov (United States)

    Monsef-Esfahani, Hamid Reza; Faramarzi, Mohammad Ali; Mortezaee, Venus; Amini, Mohsen; Rouini, Mohammad Reza

    A High-Performance Liquid Chromatography (HPLC) method was developed for determination of harmine, harmaline, harmol and harmalol in the extract of Peganum harmala seeds. The sample preparation was performed using liquid-liquid extraction. Chromatographic separation was achieved with a Tracer Excel 120 ODSA (150x4.6 mm) column, using a mixture of potassium phosphate buffer (10 mM, pH 7.0): acetonitrile (100:30; v/v) as mobile phase, in an isocratic mode at 1.5 mL min-1. UV detection (λ = 330 nm) was used. The calibration curves were linear (r2>0.998) in the concentration range of 0.5-20 μg mL-1 for all analytes. The lower limit of quantification for all analytes was 0.5 μg mL-1. The within and between day precisions in the measurement of QC samples at three tested concentrations were in the range of 0.6-10.2% for all analytes. The HPLC method is able to measure the harmala alkaloids in the plant extract. The method has suitable reproducibility, sensitivity and resolution for routine and accurate use with UV detection.

  7. Determination of Polycyclic Aromatic Hydrocarbons in Automobile Exhaust by Means of High-Performance Liquid Chromatography with Fluorescence Detection

    DEFF Research Database (Denmark)

    Nielsen, Tom

    1979-01-01

    A chromatographic method has been developed and applied to the determination of polycyclic aromatic hydrocarbons (PAHs) in particulate matter in automobile exhaust, in petrols, and in crankcase oils. The PAHs were purified from other organic compounds by thin-layer chromatography, separated by high-performance...... liquid chromatography, and measured by means of on-line fluorescence detection. The identities of the PAHs were verified by comparing the emission spectra obtained by a stop-flow technique with those of standard PAHs...

  8. An electrospray ionization-ion mobility spectrometer as detector for high- performance liquid chromatography.

    Science.gov (United States)

    Zühlke, Martin; Riebe, Daniel; Beitz, Toralf; Löhmannsröben, Hans-Gerd; Zenichowski, Karl; Diener, Marc; Linscheid, Michael W

    2015-01-01

    The application of electrospray ionization (ESI) ion mobility (IM) spectrometry on the detection end of a high-performance liquid chromatograph has been a subject of study for some time. So far, this method has been limited to low flow rates or has required splitting of the liquid flow. This work presents a novel concept of an ESI source facilitating the stable operation of the spectrometer at flow rates between 10 μL mn(-1) and 1500 μL min(-1) without flow splitting, advancing the T-cylinder design developed by Kurnin and co-workers. Flow rates eight times faster than previously reported were achieved because of a more efficient dispersion of the liquid at increased electrospray voltages combined with nebulization by a sheath gas. Imaging revealed the spray operation to be in a rotationally symmetric multijet mode. The novel ESI-IM spectrometer tolerates high water contents (≤90%) and electrolyte concentrations up to 10mM, meeting another condition required of high-performance liquid chromatography (HPLC) detectors. Limits of detection of 50 nM for promazine in the positive mode and 1 μM for 1,3-dinitrobenzene in the negative mode were established. Three mixtures of reduced complexity (five surfactants, four neuroleptics, and two isomers) were separated in the millisecond regime in stand-alone operation of the spectrometer. Separations of two more complex mixtures (five neuroleptics and 13 pesticides) demonstrate the application of the spectrometer as an HPLC detector. The examples illustrate the advantages of the spectrometer over the established diode array detector, in terms of additional IM separation of substances not fully separated in the retention time domain as well as identification of substances based on their characteristic Ims.

  9. High-performance liquid chromatography separation of unsaturated organic compounds by a monolithic silica column embedded with silver nanoparticles.

    Science.gov (United States)

    Zhu, Yang; Morisato, Kei; Hasegawa, George; Moitra, Nirmalya; Kiyomura, Tsutomu; Kurata, Hiroki; Kanamori, Kazuyoshi; Nakanishi, Kazuki

    2015-08-01

    The optimization of a porous structure to ensure good separation performances is always a significant issue in high-performance liquid chromatography column design. Recently we reported the homogeneous embedment of Ag nanoparticles in periodic mesoporous silica monolith and the application of such Ag nanoparticles embedded silica monolith for the high-performance liquid chromatography separation of polyaromatic hydrocarbons. However, the separation performance remains to be improved and the retention mechanism as compared with the Ag ion high-performance liquid chromatography technique still needs to be clarified. In this research, Ag nanoparticles were introduced into a macro/mesoporous silica monolith with optimized pore parameters for high-performance liquid chromatography separations. Baseline separation of benzene, naphthalene, anthracene, and pyrene was achieved with the theoretical plate number for analyte naphthalene as 36,000 m(-1). Its separation function was further extended to cis/trans isomers of aromatic compounds where cis/trans stilbenes were chosen as a benchmark. Good separation of cis/trans-stilbene with separation factor as 7 and theoretical plate number as 76,000 m(-1) for cis-stilbene was obtained. The trans isomer, however, is retained more strongly, which contradicts the long- established retention rule of Ag ion chromatography. Such behavior of Ag nanoparticles embedded in a silica column can be attributed to the differences in the molecular geometric configuration of cis/trans stilbenes.

  10. Vapor Pressure Determination of VM Using the Denunder-Liquid Chromatography-Mass Spectrometry Technique

    Science.gov (United States)

    2015-01-01

    obtained using a mass flow controller (MFC), rotameter, or critical orifice , with a vacuum source. The vacuum source, which is external to the...The generator was then integrated into the vapor pressure test system. The airstream entered the side arm of the generator and passed through the

  11. Quantitative profiling of retinyl esters in milk from different ruminant species by using high performance liquid chromatography-diode array detection-tandem mass spectrometry.

    Science.gov (United States)

    Rocchi, Silvia; Caretti, Fulvia; Gentili, Alessandra; Curini, Roberta; Perret, Daniela; Pérez-Fernández, Virginia

    2016-11-15

    An effective high performance liquid chromatography-diode array detection-tandem mass spectrometry (HPLC-DAD-MS/MS) analytical approach was developed for retinoid profiling in raw milk samples (cow, buffalo, ewe, and goat). The analytes were isolated by means of liquid-liquid extraction, including a "lipid freezing" step, with yields exceeding 66%. Since the positive atmospheric pressure chemical ionisation mass spectrometry (APCI-MS) detection is not completely selective, a reliable identification has been accomplished by fully separating the analytes on a tandem C18/C30 column system under non-aqueous reversed phase (NARP) chromatography conditions. After validation, different milk varieties obtained from pasture-fed animals were analysed, providing, for the first time, the retinoid composition of both buffalo's and ewe's milk. According to the literature, retinyl palmitate has been found to be the most abundant vitamin A vitamer, but retinyl oleate is the prevalent form in the caprine milk.

  12. Determination of perfluorinated compounds in packaging materials and textiles using pressurized liquid extraction with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lv, Gang; Wang, Libing; Liu, Shaocong; Li, Shufen

    2009-03-01

    A simultaneous determination method of trace amounts of perfluorinated compounds, such as perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in packaging materials and textiles, has been developed, using pressurized liquid extraction (PLE) with gas chromatography-mass spectrometry (GC/MS). The perfluorinated compounds were primarily extracted from the samples by a PLE procedure, in which the parameters were optimized by response surface methodology. The solvent was then removed by blowing nitrogen and a silylation step was carried out with N,N-bis(trimethylsilyl)trifluoroacetamide. The silylated compounds were identified and quantified by GC/MS. The proposed method was applied to determine the PFOA and PFOS in polytetrafluoroethylene packaging materials and textiles, where the detection limits of the two compounds were 1.6 and 13.9 ng mL(-1), respectively. The results showed that the concentrations of PFOA and PFOS in the packaging materials and textiles ranged from 17.5 to 45.9 and 33.7 to 81.3 ng g(-1), respectively.

  13. Purification of six lignans from the stems of Schisandra chinensis by using high-speed counter-current chromatography combined with preparative high-performance liquid chromatography.

    Science.gov (United States)

    Zhu, Lijie; Li, Bin; Liu, Xiuying; Huang, Guohui; Meng, Xianjun

    2015-11-01

    A method for the preparative purification of lignans from Schisandra chinensis was established using a combination of high-speed counter-current chromatography (HSCCC) and preparative high-performance liquid chromatography (HPLC). The crude extracts obtained from S. chinensis by using 70% ethanol were separated on a macroporous resin column and then eluted with a graded ethanol series. A two-phase solvent system consisting of n-hexane-ethyl acetate-methanol-water (1:1:1:1, v/v) was used for HSCCC, and a mobile phase of acetonitrile-water (50:50, v/v) was used for preparative HPLC. The results obtained using HSCCC were compared with those obtained using preparative HPLC, and their advantages were further integrated to improve the separation efficiency. Six known lignans were identified by electrospray ionisation mass spectrometry and (1)H nuclear magnetic resonance (NMR) and (13)C NMR analyses; the purities of all the compounds were more than 91%.

  14. Separation of three anthraquinone glycosides including two isomers by preparative high-performance liquid chromatography and high-speed countercurrent chromatography from Rheum tanguticum Maxim. ex Balf.

    Science.gov (United States)

    Chen, Tao; Li, Hongmei; Zou, Denglang; Liu, Yongling; Chen, Chen; Zhou, Guoying; Li, Yulin

    2016-08-01

    Anthraquinone glycosides, such as chrysophanol 1-O-β-d-glucoside, chrysophanol 8-O-β-d-glucoside, and physion 8-O-β-d-glucoside, are the accepted important active components of Rheum tanguticum Maxim. ex Balf. due to their pharmacological properties: antifungal, antimicrobial, cytotoxic, and antioxidant activities. However, an effective method for the separation of the above-mentioned anthraquinone glycosides from this herb is not currently available. Especially, greater difficulty existed in the separation of the two isomers chrysophanol 1-O-β-d-glucoside and chrysophanol 8-O-β-d-glucoside. This study demonstrated an efficient strategy based on preparative high-performance liquid chromatography and high-speed countercurrent chromatography for the separation of the above-mentioned anthraquinone glycosides from Rheum tanguticum Maxim.ex Balf.

  15. Hydrocarbon group type determination in jet fuels by high performance liquid chromatography

    Science.gov (United States)

    Antoine, A. C.

    1977-01-01

    Results are given for the analysis of some jet and diesel fuel samples which were prepared from oil shale and coal syncrudes. Thirty-two samples of varying chemical composition and physical properties were obtained. Hydrocarbon types in these samples were determined by fluorescent indicator adsorption (FIA) analysis, and the results from three laboratories are presented and compared. Recently, rapid high performance liquid chromatography (HPLC) methods have been proposed for hydrocarbon group type analysis, with some suggestion for their use as a replacement of the FIA technique. Two of these methods were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.

  16. Analysis of lipophilic pigments from a phototrophic microbial mat community by high performance liquid chromatography

    Science.gov (United States)

    Palmisano, A. C.; Cronin, S. E.; Des Marais, D. J.

    1988-01-01

    As assay for lipophilic pigments in phototrophic microbial mat communities using reverse phase-high performance liquid chromatography was developed which allows the separation of 15 carotenoids and chloropigments in a single 30 min program. Lipophilic pigments in a laminated mat from a commercial salina near Laguna Guerrero Negro, Baja California Sur, Mexico reflected their source organisms. Myxoxanthophyll, echinenone, canthaxanthin, and zeaxanthin were derived from cyanobacteria; chlorophyll c, and fucoxanthin from diatoms; chlorophyll a from cyanobacteria and diatoms; bacteriochlorophylls a and c, bacteriophaeophytin a, and gamma-carotene from Chloroflexus spp.; and beta-carotene from a variety of phototrophs. Sensitivity of detection was 0.6-6.1 ng for carotenoids and 1.7-12 ng for most chloropigments. This assay represents a significant improvement over previous analyses of lipophilic pigments in microbial mats and promises to have a wider application to other types of phototrophic communities.

  17. Simultaneous Determination of Five Components Including Acetaminophen by Reversed-phase High Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    ZHANG Li-qing; WU Xiao-hua; LU Ying; WANG Xia

    2004-01-01

    High performance liquid chromatography with a C18 reverse-phase column was used to separatethe five components in cough syrup, including acetaminophen, p-aminophenol, caffeine, chlorphenamine maleateand guaifenesin. The mobile phase consists of 15wi% acetonitrile, 0.004mol/L sodium heptyl sulfonate,0.03 mole/L potassium di- hydrogen phosphate and triethylamine ( volume ratio 13: 40: 44: 3), the pH of which isadjusted to 3.0 by phosphoric acid. The contents of the five components are analyzed on an ultraviolet spectropho-tometer at 254nm, with a flow rate of 0.4mL/min. The results show that the calibration curves are linear in acertain range. The average recovery of five components is between 96.31% and 102.3% .

  18. Determination of free urinary cortisol in cushing's syndrome using reversed-phase high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Eduardo Kinio Sugawara

    2010-01-01

    Full Text Available Determination of free urinary cortisol is a test of choice in the diagnosis of Cushing's syndrome. In this study, cortisol was quantified using reversed-phase high-performance liquid chromatography (RP-HPLC in urine samples previously extracted with ether and using triamcinolone acetonide as internal standard (IS. A BDS-Hypersil-C18® column, water-acetonitrile (72:28; v/v, with a flow rate of 1.0 mL/min and detection at 243 nm were used. This method showed to be both effective and efficient, with sensitivity and linearity ranging from 2.50 to 150 μg/L, and can be used in substitution to the radioimmunoassay technique within this concentration range.

  19. High performance liquid chromatography study of complex oxygenated alkane mixtures from organic aerosols

    Science.gov (United States)

    Kalafut-Pettibone, Alicia J.; Klems, Joseph P.; McGivern, W. Sean

    2013-05-01

    The composition of secondary organic aerosol particles is of primary importance both in identifying particle sources and in determining physical parameters, such as cloud condensation nucleus propensity. Further, measurements of composition are valuable in determining the chemistry of formation and aging. In this work, we describe the application of a recently-developed derivatization technique to a complex synthetic organic aerosol derived from the photolysis of 1-iodooctane. The technique utilizes high-performance liquid chromatography (HPLC) coupled to both ultravioletvisible (UV/VIS) spectroscopy and tandem mass spectrometry (MS-MS) to determine the overall distribution of hydroxyl (OH), non-acid carbonyl (C=O), and carboxylic acid (COOH) moieties as well as the specific identities of chromatographically separated products. This composition data will then be used to constrain models of the particle formation mechanisms.

  20. Determination of triazine herbicides in milk by cloud point extraction and high-performance liquid chromatography.

    Science.gov (United States)

    Liu, Tiantian; Cao, Peng; Geng, Jinpei; Li, Jinqiang; Wang, Mingzhen; Wang, Minglin; Li, Xiaoyu; Yin, Dalu

    2014-01-01

    High-performance liquid chromatography with UV detection was used to detect four triazines in milk. An efficient pretreatment method known as cloud point extraction (CPE) was proposed for extracting and preconcentrating analytes. The parameters of CPE including surfactant type and concentration, electrolyte, sample pH, incubation temperature and duration were investigated. Under optimal conditions, satisfying recoveries in the range of 70.5-96.9% were achieved for four triazines. The limits of detection ranged from 6.79 to 11.19μg L(-1). The linear range of quantitation for the four triazines was 50-2000μg L(-1), and the correlation coefficients of the calibration curves were all 0.9999. The results demonstrated that the proposed method was efficient and reliable for the determination of triazine herbicides in milk samples.

  1. Measurement of serum pralidoxime methylsulfate (Contrathion) by high-performance liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Houzé, Pascal; Borron, Stephen W; Scherninski, François; Bousquet, Bernard; Gourmel, Bernard; Baud, Frédéric

    2005-01-05

    Pralidoxime methylsulfate (Contrathion) is widely used to treat organophosphate poisoning. Despite animal and human studies, the usefulness of Contrathion therapy remains a matter of debate. Therapeutic dosage regimens need to be clarified and availability of a reliable method for plasma pralidoxime quantification would be helpful in this process. We here describe a high-performance liquid chromatography technique with electrochemical detection to measure pralidoxime concentrations in human serum using guanosine as an internal standard. The assay was linear between 0.25 and 50 microg mL(-1) with a quantification limit of 0.2 microg mL(-1). The analytical precision was satisfactory, with variation coefficients lower 10%. This assay was applied to the analysis of a serum from an organophosphorate poisoned patient and treated by Contrathion infusions (100 and 200 mg h(-1)) after a loading dose (400 mg).

  2. A validated new method for nevirapine quantitation in human plasma via high-performance liquid chromatography.

    Science.gov (United States)

    Silverthorn, Courtney F; Parsons, Teresa L

    2006-01-01

    A fully validated and clinically relevant assay was developed for the assessment of nevirapine concentrations in neonate blood plasma samples. Solid-phase extraction with an acid-base wash series was used to prepare subject samples for analysis. Samples were separated by high performance liquid chromatography and detected at 280 nm on a C8 reverse-phase column in an isocratic mobile phase. The retention times of nevirapine and its internal standard were 5.0 and 6.9 min, respectively. The method was validated by assessment of accuracy and precision (statistical values 0.996) and the average recovery was 93% (n = 18). The lower limit of quantification (relative standard deviation <20%) was determined to be 25 ng/mL for 50 microL of plasma, allowing detection of as little as 1.25 ng of nevirapine in a sample. This value represents an increase in sensitivity of up to 30-fold over previously published methods.

  3. Development of High Performance Liquid Chromatography and Mass Spectrometry:a Key Engine of TCM Modernization

    Institute of Scientific and Technical Information of China (English)

    Zheng-Xiang Zhang; Xue Qiao; Min Ye; Man-Yu Zhang; Yue Song; Tao Bo

    2015-01-01

    Traditional Chinese Medicine (TCM) has been popular for thousand years in prevention and treatment of chronic diseases synergistically with Western medicine while producing mild healing effects and lower side effects. Although many TCMs have been proven effective by modern pharmacological studies and clinical trials, their bioactive constituents and the remedial mechanisms are still not well understood. Researchers have made great efforts to explore the real theory of TCM for many years with different strategies. Development of high performance liquid chromatography (HPLC) and mass spectrometry within recent decade can provide scientists with robust technologies for disclosing the mysterious mask of TCM. In this paper, important innovations of HPLC and mass spectrometry are reviewed in the application of TCM analysis from single compound identification to metabolomic strategy.

  4. High-performance liquid chromatography determination of dapsone, monoacetyldapsone, and pyrimethamine in filter paper blood spots

    DEFF Research Database (Denmark)

    Rønn, A M; Lemnge, M M; Angelo, H R

    1995-01-01

    A high-performance liquid chromatography method for the simultaneous analysis of dapsone (DDS), the major metabolite of DDS, monoacetyldapsone (MADDS), and pyrimethamine (PYR) was modified for capillary blood samples obtained by finger prick and dried on filter paper. Limit of quantitation using...... 150 microliters whole blood dried on filter paper was found to be 20 ng/ml for DDS and PYR and 15 ng/ml for MADDS (precision ... paper method and the original whole-blood method was almost comparable. Standardization could therefore be obtained by the more simple whole-blood method. Dried filter paper samples stored at 19-22 degrees C were stable for months and for 2 weeks stored at 35 degrees C. The concentrations...

  5. Development of N-ferrocenyl(benzoyl)amino-acid esters stationary phase for high performance liquid chromatography.

    Science.gov (United States)

    Zhou, Xiaohua; Li, Xiaole; Cao, Aijuan; Lijun, Qiao; Yu, Ajuan; Zhang, Shusheng; Wu, Yangjie

    2015-11-01

    A new stationary phase for high-performance liquid chromatography was prepared by covalently bonding N-ferrocenyl(benzoyl)amino-acid esters (L(1)) onto silica gel using 3-aminopropyltriethoxysilane as coupling reagent. The structure of new material was characterized by infrared spectroscopy, elemental analysis and thermogravimetric analysis. The chromatographic behavior of the phase was illustrated in reversed-phase (RP) and normal-phase (NP) modes using polycyclic aromatic hydrocarbons (PAHs), aromatics positional isomers, amines, 5-nitroimidazoles, organophosphorus pesticides and phenols as probes. Multiple mechanisms including hydrophobic, hydrogen bonding, π-π, dipole-dipole, charge-transfer and acid-base equilibrium interactions are involved. Thus, multi-interaction mechanisms and mixed-mode separation of the new phase can very likely guarantee its excellent chromatographic performance for the analysis of complex samples. The L(1) AminoSil column was successfully employed for the analysis of organophosphorus pesticides in vegetable.

  6. Determination of primary amino acids in wines by high performance liquid magneto-chromatography.

    Science.gov (United States)

    Barrado, E; Rodriguez, J A; Castrillejo, Y

    2009-05-15

    Eight amino acids (ethanolamine, glycine, alanine, beta-aminobutyric acid, leucine, methionine, histidine and asparagine) were identified and quantified in Spanish wines by high performance liquid magneto-chromatography (HPLMC) with UV-V spectrophotometry. For this method, the amino acids are first complexed with mono(1,10-phenanthroline)-Cu(II) to confer them paramagnetic properties, and then separated by application of a low magnetic field intensity (5.5 mT) to the stationary phase contained in the chromatographic column. Principal components analysis of the results obtained grouped together the wine samples according to their denomination of origin: "Ribera del Duero", "Rueda" or "Rioja" (Spain). Through cluster analysis, a series of correlations was also observed among certain amino acids, and between these groupings and the type of wine. These clusters were found to reflect the role played by the amino acids as primary or secondary nutrients for the bacteria involved in alcoholic and malolactic fermentation.

  7. Tritium isotope effect in high-performance liquid chromatography of eicosanoids

    Energy Technology Data Exchange (ETDEWEB)

    Do, U.H.; Lo, S.-L.; Iles, J.; Rosenberger, T.; Tam, P.; Hong, Y.; Ahern, D. [DuPont, NEN Products, Boston (United States). Lipids Group

    1994-07-01

    A significant difference in retention time between unlabeled and the corresponding multi-tritium-labeled eicosanoid has been observed in the high performance liquid chromatography (HPLC) analysis of 11 eicosanoids. Variations in retention time range from 3-7%, depending on the separation conditions as well as the number and position of the tritium substitution. Multi-tritium-labeled eicosanoids were eluted earlier than the corresponding unlabeled eicosanoid in reversed phase HPLC, whereas no isotope effect was seen with {sup 14}C- and {sup 3}H{sub 2}-eicosanoids. Considerations must be given to this tritium isotope effect whenever both multi-tritium-labeled and unlabeled eicosanoids are used for HPLC cochromatography or recovery studies. (author).

  8. Detection of cheese whey and caseinomacropeptide in fermented milk beverages using high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    E.H.P. Andrade

    2014-06-01

    Full Text Available Cheese whey level and caseinomacropeptide (CMP index of fermented milk beverages added with four levels of cheese whey (0, 10, 20, and 40% and stored at 8-10oC for 0, 7, 14 and 21 days were determined by high performance liquid chromatography-gel filtration (HPLC-GF. Additionally, the interference of the starter culture and the storage time on the detection of cheese whey and CMP were investigated. Refrigerated storage up to 21 days did not affect (P>0.05 cheese whey and CMP amounts in milk (0% of cheese whey and in fermented milk beverages added with 10 and 20% of cheese whey (P>0.05. However, cheese whey and CMP amounts were higher than expected (P<0.05 in fermented milk beverages added with 40% of cheese whey and stored for 21 days.

  9. Postcolumn photolysis of pesticides for fluorometric determination by high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Miles, C.J.; Moye, H.A.

    1988-02-01

    A high-performance liquid chromatography postcolumn reaction detector that employs UV photolysis with an optional reaction by using o-phthalaldehyde-2-mercaptoethanol (OPA-MERC) followed by fluorescence detection was found to be useful for several classes of pesticides. In the presence of the OPA-MERC reagent, most carbamates, carbamoyl oximes, carbamothioic acids, and substituted ureas gave a sensitive response while the response of dithiocarbamates, phenylamides, and phenylcarbamates varied. The response of most of the pesticides tested was significantly affected by the solvent used. Method detection limits for aldicarb sulfoxide, aldicarb, propoxur, thiram, and neburon in ground water were 2.5, 2.3, 3.3, 3.8, and 2.0 ..mu..g/L, respectively. In the absence of OPA-MERC reagent, several of the substituted aromatic compounds also gave strong fluorescence after photolysis. This detector is applicable to a broad range of nitrogenous pesticides.

  10. A high performance liquid chromatography method for determination of furfural in crude palm oil.

    Science.gov (United States)

    Loi, Chia Chun; Boo, Huey Chern; Mohammed, Abdulkarim Sabo; Ariffin, Abdul Azis

    2011-09-01

    A modified steam distillation method was developed to extract furfural from crude palm oil (CPO). The collected distillates were analysed using high performance liquid chromatography (HPLC) coupled with an ultraviolet diode detector at 284nm. The HPLC method allowed identification and quantification of furfural in CPO. The unique thermal extraction of CPO whereby the fresh fruit bunches (FFB) are first subjected to steam treatment, distinguishes itself from other solvent-extracted or cold-pressed vegetable oils. The presence of furfural was also determined in the fresh palm oil from FFB (without undergoing the normal extraction process), palm olein, palm stearin, olive oil, coconut oil, sunflower oil, soya oil and corn oil. The chromatograms of the extracts were compared to that of standard furfural. Furfural was only detected in CPO. The CPO consignments obtained from four mills were shown to contain 7.54 to 20.60mg/kg furfural.

  11. Determination of Sex Hormones in Antler Velvet by High Performance Liquid Chromatography Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    LU Chun-mei; WANG Ming-tai; MU Jun; BAI Yu-ping; DU Jian-shi; ZHANG Han-qi; WANG Jian-wei

    2012-01-01

    Eighteen sex hormones in antler velvet were determined by high performance liquid chromatography tandem mass spectrometry.The solid phase extraction was applied to eliminating the matrix effect.The experimental conditions were examined and optimized.Under the optimal conditions,the proposed method provides the good linearities and determination limits(0.2-1.0 μg/kg)of the analytes investigated.The recoveries ranging from 72.3% to 149.5% were obtained for the target analytes at two concentration levels.This method was applied to the determination of eighteen sex hormones in different kinds of antler velvet samples and the obtained results are satisfactory.The results indicate that the proposed method is suitable for the determination of sex hormones in antler velvet samples.

  12. Determination of captopril by high-performance liquid chromatography with direct electrogenerated chemiluminescence

    Science.gov (United States)

    Sun, Yonghua; Zhang, Zhujun; Zhang, Xinfeng

    2013-03-01

    Captopril exhibit electrogenerated chemiluminescence (ECL) in NaNO3 solution when constant current is exerted. Based on this observation, a direct ECL method coupled with high-performance liquid chromatography (HPLC) separation is developed for determination of captopril in human serum. Factors affected the ECL emission are investigated. Under the optimal conditions, the ECL intensity has a linear relationship with the concentration of captopril in the range of 4.0 × 10-6-2.0 × 10-3 g mL-1 and the detection limit is 2 × 10-6 g mL-1 (S/N = 3). Compared with the common electrogenerated chemiluminescence experiments, the developed method need no any other fluorescence additives.

  13. Quantitative determination of acetaminophen, phenylephrine and carbinoxamine in tablets by high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Carina de A. Bastos

    2009-01-01

    Full Text Available An alternative methodology for analysis of acetaminophen (Ace, phenylephrine (Phe and carbinoxamine (Car in tablets by ion-pair reversed phase high performance liquid chromatography was validated. The pharmaceutical preparations were analyzed by using a C18 column (5 μm, 300 mm, 3.9 mm and mobile phase consisting of 60% methanol and 40% potassium monobasic phosphate aqueous solution (62.46 mmol L-1 added with 1 mL phosphoric acid, 0.50 mL triethylamine and 0.25 g sodium lauryl sulfate. Isocratic analysis was performed under direct UV detection at 220 nm for Phe and Car and at 300 nm for Ace within 5 min.

  14. High-performance liquid chromatography for determination of α-tocopherol in vegetables

    Directory of Open Access Journals (Sweden)

    Marcin Horbowicz

    2013-12-01

    Full Text Available A simple method for the determination of α-tocopherol in vegetables is described. The procedure consists of the following steps: saponification, extraction, silica-column clean-up, and high-performance liquid chromatography. Elution time for D, L-α-tocopherol was 9.0 min using a Zorbax Sil (250 x 4.6 mm column and an isocratic mobile phase of hexane-methanol (99.3 + 0.7, with a flow rate of 1 ml/min, and detection at 292 nm using a variable UV detector. The average recovery of α-tocopherol was 91.2%, and the minimum detectable amount was 0.1 mg/100 g of fresh vegetable tissue. This method is comparable to gas-chromatographic determination of α-tocopherol, but has fewer analytical steps and gives more reproducible results.

  15. Development and comparison of two dispersive liquid-liquid microextraction techniques coupled to high performance liquid chromatography for the rapid analysis of bisphenol A in edible oils.

    Science.gov (United States)

    Liu, Shuhui; Xie, Qilong; Chen, Jie; Sun, Janzhi; He, Hui; Zhang, Xiaoke

    2013-06-21

    In this study, two novel sample extraction methods for the analysis of bisphenol A (BPA) in edible oils were developed by using liquid-liquid extraction followed by a dispersive liquid-liquid microextraction (LLE-DLLME) and reversed-phase dispersive liquid-liquid microextraction (RP-DLLME). RP-DLLME showed a superior characteristic over LLE-DLLME and other previously reported procedures because of its easy operation, short extraction time, high sensitivity, low organic solvent consumption and waste generation. The optimized extraction conditions of RP-DLLME for 1.0 g of edible oil diluted in 4 mL of n-hexane were: extractant, 100 μL 0.2 M sodium hydroxide solution (80% methanol, v/v); extraction time, 1 min; centrifugation, 3 min. The determination of BPA was carried out by high performance liquid chromatography coupled with a DAD detector. The method offered excellent linearity over a range of 0.010-0.5 μg g(-1) with a correlation coefficient of r>0.997. Intra-day and inter-day repeatability values expressed as relative standard deviation were 1.9% and 5.9%, respectively. The quantitation limit and detection limit were 6.3 and 2.5 ng g(-1). The target analyte was detected in 5 out of 16 edible oil samples. The recovery rates in real samples ranged from 89.5 to 99.7%.

  16. High Performance Thin Layer Chromatography.

    Science.gov (United States)

    Costanzo, Samuel J.

    1984-01-01

    Clarifies where in the scheme of modern chromatography high performance thin layer chromatography (TLC) fits and why in some situations it is a viable alternative to gas and high performance liquid chromatography. New TLC plates, sample applications, plate development, and instrumental techniques are considered. (JN)

  17. Chromatographic performance of synthetic polycrystalline diamond as a stationary phase in normal phase high performance liquid chromatography.

    Science.gov (United States)

    Peristyy, Anton; Paull, Brett; Nesterenko, Pavel N

    2015-04-24

    The chromatographic properties of high pressure high temperature synthesised diamond (HPHT) are investigated in normal phase mode of high performance liquid chromatography. Purified nonporous irregular shape particles of average particles size 1.2 μm and specific surface area 5.1 m(2) g(-1) were used for packing 100×4.6 mm ID or 50×4.6 mm ID stainless steel columns. The retention behaviour of several classes of compounds including alkyl benzenes, polyaromatic hydrocarbons (PAH), alkylphenylketones, phenols, aromatic acids and bases were studied using n-hexane-2-propanol mixtures as mobile phase. The results are compared with those observed for microdispersed sintered detonation nanodiamond (MSDN) and porous graphitic carbon (PGC). HPHT diamond revealed distinctive separation selectivity, which is orthogonal to that observed for porous graphitic carbon; while selectivities of HPHT diamond and microdispersed sintered detonation nanodiamonds are similar. Owing to non-porous particle nature, columns packed with high pressure high temperature diamond exhibited excellent mass transfer and produce separations with maximum column efficiency of 128,200 theoretical plates per meter.

  18. Selective pressurized liquid extraction of estrogenic compounds in soil and analysis by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zhang, Zulin; Rhind, Stewart M; Kerr, Christine; Osprey, Mark; Kyle, Carol E

    2011-01-24

    A selective pressurized liquid extraction (SPLE) method, followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous extraction and clean-up of estrone (E1), 17β-estradiol (E2), 17α-ethynylestradiol (EE2), estriol (E3) and bisphenol A (BPA) from soil samples is described. The on-line clean-up of soil by SPLE was achieved using different organic matter retainers, including silica, alumina and Florisil, the most effective being silica. Thus, different amounts of silica, in conjunction with different extraction solvents (acetone, ethyl acetate, isohexane and dichloromethane), either alone or in combination, were used to extract the target chemicals from spiked soil samples. It was shown that 3g silica resulted in satisfactory rates of recovery of target compounds and acetone:dichloromethane (1:3, v/v) was efficient in extracting and eluting estrogenic compounds for SPLE. Variables affecting the SPLE efficiency, including temperature and pressure were studied; the optimum parameters were 60°C and 1500 psi, respectively. The limits of detection (LODs) of the proposed method were 0.02-0.37 ng g(-1) for the different estrogenic chemicals studied. The outputs using the proposed method were linear over the range from 0.1 to 120 ng g(-1) for E1, E2, EE2, 0.2-120 ng g(-1) for E3, and 0.5-120 ng g(-1) for BPA. The optimized method was further verified by performing spiking experiments in natural soil matrices; good rates of recovery and reproducibility were achieved for all selected compounds and the method was successfully applied to soil samples from Northeast Scotland, for the determination of the target compounds.

  19. Quartz Tuning Fork Pressure Gauge for High-Pressure Liquid Helium

    Science.gov (United States)

    Botimer, J.; Velasco, A.; Taborek, P.

    2017-01-01

    We have measured the quality factor Q and the frequency f of a 32-kHz quartz tuning fork immersed in liquid ^4He between 0.9 and 3.0 K, over pressures ranging from the saturated vapor pressure to ≈ 25 atm. At constant pressure, as a function of temperature, the quality factor and frequency have strong features related to the temperature dependence of the superfluid fraction. At constant temperature, Q depends on the superfluid fraction, while the frequency is a smooth function of pressure. The behavior is explained using a simple hydrodynamic model. The liquid helium viscosity is obtained from measured values of Q, and together with tabulated values of the helium density as a function of pressure and temperature, the frequency shift can be parameterized as a function of temperature and pressure. The observed sensitivity is ≈ 7.8 Hz/atm. The quartz tuning fork provides a compact low power method of measuring the pressure in the bulk liquid.

  20. Ultrafiltration liquid chromatography combined with high-speed countercurrent chromatography for screening and isolating potential α-glucosidase and xanthine oxidase inhibitors from Cortex Phellodendri.

    Science.gov (United States)

    Li, Sainan; Liu, Chunming; Guo, Liping; Zhang, Yuchi; Wang, Jing; Ma, Bing; Wang, Yueqi; Wang, Yumeng; Ren, Junqi; Yang, Xiaojing; Qin, Yao; Tang, Ying

    2014-09-01

    Cortex Phellodendri is a typical Chinese herb with a large number of alkaloids existing in all parts of it. The most common methods for screening and isolating alkaloids are mostly labor intensive and time consuming. In this study, a new assay based upon ultrafiltration liquid chromatography was developed for the rapid screening of ligands for α-glucosidase and xanthine oxidase. The C. Phellodendri extract was found to contain two alkaloids with both α-glucosidase- and xanthine oxidase binding activities and one lactone with α-glucosidase-binding activity. Subsequently, with the help of high-speed countercurrent chromatography, the specific binding ligands including palmatine, berberine, and obaculactone with purities of 97.38, 96.12, and 96.08%, respectively, were successfully separated. An optimized low-toxicity two-phase solvent system composed of ethyl acetate/n-butanol/ethanol/water (3.5:1.7:0.5:5, v/v/v/v) was used to isolate the three compounds mentioned above from C. Phellodendri. The targeted compounds were identified by liquid chromatography coupled with mass spectrometry and NMR spectroscopy. Therefore, ultrafiltration liquid chromatography combined with high-speed countercurrent chromatography is not only a powerful tool for screening and isolating α-glucosidase and xanthine oxidase inhibitors in complex samples but is also a useful platform for discovering bioactive compounds for the prevention and treatment of diabetes mellitus and gout.

  1. Comprehensive sample analysis using high performance liquid chromatography with multi-detection

    Energy Technology Data Exchange (ETDEWEB)

    Pravadali, Sercan [Australian Centre for Research on Separation Sciences (ACROSS), School of Science and Health, University of Western Sydney (Parramatta), NSW 1797 (Australia); Bassanese, Danielle N.; Conlan, Xavier A.; Francis, Paul S.; Smith, Zoe M.; Terry, Jessica M. [Centre for Chemistry and Biotechnology, School of Life and Environmental Sciences, Deakin University, Victoria 3216 (Australia); Shalliker, R. Andrew, E-mail: R.Shalliker@uws.edu.au [Australian Centre for Research on Separation Sciences (ACROSS), School of Science and Health, University of Western Sydney (Parramatta), NSW 1797 (Australia)

    2013-11-25

    Graphical abstract: -- Highlights: •Detection selectivity was assessed with 6 detection modes. •Natural samples show great diversity in detection selectivity. •Complex samples require evaluation using a multifaceted approach to detection. •23/30 known compounds (detected by MS) detected by chemiluminescence, DPPH and UV. -- Abstract: Herein we assess the separation space offered by a liquid chromatography system with an optimised uni-dimensional separation for the determination of the key chemical entities in the highly complex matrix of a tobacco leaf extract. Multiple modes of detection, including UV–visible absorbance, chemiluminescence (acidic potassium permanganate, manganese(IV), and tris(2,2′-bipyridine)ruthenium(III)), mass spectrometry and DPPH radical scavenging were used in an attempt to systematically reduce the data complexity of the sample whilst obtaining a greater degree of molecule-specific information. A large amount of chemical data was obtained, but several limitations in the ability to assign detector responses to particular compounds, even with the aid of complementary detection systems, were observed. Thirty-three compounds were detected via MS on the tobacco extract and 12 out of 32 compounds gave a peak height ratio (PHR) greater than 0.33 on one or more detectors. This paper serves as a case study of these limitations, illustrating why multidimensional chromatography is an important consideration when developing a comprehensive chemical detection system.

  2. Determination of clomazone residues in soybean and soil by high performance liquid chromatography with DAD detection.

    Science.gov (United States)

    Hu, Jiye; Cao, Di; Deng, Zhubo

    2011-04-01

    A simple analysis method to detect clomazone residues in soybean and soil was developed using solid phase extraction coupled with high performance liquid chromatography with diode-array detection. The pesticide residues present in soybean and soil matrices were extracted with methanol-water and extracts purified with Florisil cartridges. The analytes from soybean and soil matrix were eluted with petroleum ether-acetic ether (10 mL, 95:5, v/v) and petroleum ether-acetic ether (2 mL, 95:5, v/v), respectively. The overall recovery of fortified soybean and soil at the levels of 0.01, 0.1 and 0.5 mg/kg ranged from 89.75% to 106.6%, and the coefficients of variation (CV) ranged from 1.68% to 4.93% (n = 3). The limit of quantification (LOQ) is 0.01 mg/kg. This method has been applied to the analysis of clomazone in real samples of soybean and soil. The dissipation of residue over the time in soil coincided with C = 1.189e(-0.0926t ) and the half-lives (T(1/2)) was 7.48 days. The final residue in soybean was lower than 0.01 mg/kg at harvest time. Direct confirmation of the analyte in real samples was achieved by gas chromatography-mass spectrometry.

  3. Determination of Acrylamide Metabolite ,Mercapturic Aicd by High Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    WUYi-Qun; YUAi-Ru; 等

    1993-01-01

    A HPLC Assay was developed to indentify and measure the metabolite of acrylamide,mercapturic acid,N-Acetyl-s-(propionamide)-cyteine(APC)in urine O-phthalaldehyde (OPA)was utilized as a precolumm derivatizing agent in the assay.This derivative was isolated with a good selectivity by high performance liquid chromatography(HPLC)employing reversed phase ODS columns.The quantiation of the mercapturic acid derivative was reproducible and with a detection limit of 1 pmol.The average coefficient of variation for the runs carried out on the same day was approximately 4.6% at the range of 80-160μmol·l-1 of APC,and the mean analytical recovery from urine samples was 94%.The metabolite of urine of workers exposed to acrylamide was identified as N-acetyl-s-(propionamide)-cysteine by HPLC chromatography and fluorescence scan and HPLC-Mass spectra.All results were identical with the authentic synthesized compound.

  4. Quantitation of clobazam in human plasma using high-performance liquid chromatography.

    Science.gov (United States)

    Knapp, J; Bokník, P; Gumbinger, H G; Linck, B; Lüss, H; Müller, F U; Schmitz, W; Vahlensieck, U; Neumann, J

    1999-05-01

    A rapid and simple reversed-phase high-performance liquid chromatographic (HPLC) method for the determination of clobazam concentrations in human blood samples is developed and validated. Solid-phase column extraction is performed to clean up blood samples before running the analytical HPLC system. The chromatography is isocratic with a mobile phase consisting of acetonitrile (20%, v/v), methanol (23%, v/v), and 0.1 M potassium hydrogen phosphate buffer (pH 3.6; 57%, v/v) at a constant flow rate of 2 mL/min. Clobazam is detected at 226 nm. Chromatography is completed within less than 25 min. The recovery rate is greater than 95% and linear over a wide range of drug concentrations. The intra-assay coefficient of variation percentage varies between 4.3 and 12. This method is used for therapeutic drug monitoring in patients undergoing antiepileptic therapy with clobazam. Plasma levels of clobazam ranged from 21 to 663 ng/mL. Other antiepileptic compounds, such as clonazepam and phenobarbital, did not interfere with the detection of clobazam.

  5. Comparison of microemulsion electrokinetic chromatography with high-performance liquid chromatography for fingerprint analysis of resina draconis.

    Science.gov (United States)

    Cao, Yuhua; Gong, Wenjun; Li, Nan; Yin, Changna; Wang, Yun

    2008-11-01

    Microemulsion electrokinetic chromatography (MEEKC) has been developed for fingerprint analysis of resina draconis, a substitute for sanguis draconis in the Chinese market. The microemulsion as the running buffer was made up of 3.3% (w/v) sodium dodecyl sulfate (SDS), 6.6% (w/v) n-butanol, 0.8% (w/v) n-octane, and 10 mmol/L sodium tetraborate buffer (pH 9.2), which was also used as the solvent for ultrasonic extraction of both water- and fat-soluble compounds in the traditional Chinese medicine samples. Four batches of resina draconis obtained from different pharmaceutical factories located in different geographic regions were used to establish the electrophoretic fingerprint. MEEKC was performed using a Beckman PACE/MDQ system equipped with a diode-array detector and with monitoring at 280 nm. The fingerprint of resina draconis comprised 27 common peaks within 100 min. The relative standard deviations of the relative migration time of these common peaks were less than 2.1%. Through repetitive injection of the sample solution six times in 24 h, all relative standard deviations of the migration time and peak area of loureirin A and loureirin B were less than 2.5 and 3.8%, which demonstrated that the method had good stability and reproducibility. The relative peak areas of these common peaks in the electropherograms of four batches of resina draconis were processed with two mathematical methods, the correlation coefficient and the interangle cosine, to valuate the similarity. The values of the similarity degree of all samples were more than 0.91, which showed resina draconis samples from different origins were consistent. On the other hand, high-performance liquid chromatography (HPLC) coupled with photodiode-array detection was also applied to establish the fingerprint of resina draconis. The samples were separated with a LiChrospher C(18) column using acetonitrile (solvent A) and water containing 0.1% H(3)PO(4) (solvent B) as the mobile phase in linear gradient

  6. Parallel segmented outlet flow high performance liquid chromatography with multiplexed detection

    Energy Technology Data Exchange (ETDEWEB)

    Camenzuli, Michelle [Australian Centre for Research on Separation Science (ACROSS), School of Science and Health, University of Western Sydney (Parramatta), Sydney, NSW (Australia); Terry, Jessica M. [Centre for Chemistry and Biotechnology, School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3216 (Australia); Shalliker, R. Andrew, E-mail: r.shalliker@uws.edu.au [Australian Centre for Research on Separation Science (ACROSS), School of Science and Health, University of Western Sydney (Parramatta), Sydney, NSW (Australia); Conlan, Xavier A.; Barnett, Neil W. [Centre for Chemistry and Biotechnology, School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3216 (Australia); Francis, Paul S., E-mail: paul.francis@deakin.edu.au [Centre for Chemistry and Biotechnology, School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3216 (Australia)

    2013-11-25

    Graphical abstract: -- Highlights: •Multiplexed detection for liquid chromatography. •‘Parallel segmented outlet flow’ distributes inner and outer portions of the analyte zone. •Three detectors were used simultaneously for the determination of opiate alkaloids. -- Abstract: We describe a new approach to multiplex detection for HPLC, exploiting parallel segmented outlet flow – a new column technology that provides pressure-regulated control of eluate flow through multiple outlet channels, which minimises the additional dead volume associated with conventional post-column flow splitting. Using three detectors: one UV-absorbance and two chemiluminescence systems (tris(2,2′-bipyridine)ruthenium(III) and permanganate), we examine the relative responses for six opium poppy (Papaver somniferum) alkaloids under conventional and multiplexed conditions, where approximately 30% of the eluate was distributed to each detector and the remaining solution directed to a collection vessel. The parallel segmented outlet flow mode of operation offers advantages in terms of solvent consumption, waste generation, total analysis time and solute band volume when applying multiple detectors to HPLC, but the manner in which each detection system is influenced by changes in solute concentration and solution flow rates must be carefully considered.

  7. High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

    Science.gov (United States)

    Haddad, Paul; And Others

    1983-01-01

    Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

  8. High throughput pyrogenic carbon (biochar) characterisation and quantification by liquid chromatography

    NARCIS (Netherlands)

    Cerqueira, W.V.; Rittl, T.F.; Novotny, E.H.; Pereira Netto, A.D.

    2015-01-01

    Characterisation and quantification of the carbonaceous polyaromatic structure of pyrogenic carbon (PyC) are of paramount importance to evaluate the role of PyC in soil carbon sequestration. A new method of rapid resolution liquid chromatography with UV diode array detection (RRLC-UV-DAD) was dev

  9. Low density solvent-based dispersive liquid-liquid microextraction for the determination of synthetic antioxidants in beverages by high-performance liquid chromatography.

    Science.gov (United States)

    Çabuk, Hasan; Köktürk, Mustafa

    2013-01-01

    A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL(-1). The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

  10. High Performance Liquid Chromatography Tandem Mass Spectrometry Measurement of Bimatoprost, Latanoprost and Travoprost in Eyelash Enhancing Cosmetic Serums

    Directory of Open Access Journals (Sweden)

    Emilia Marchei

    2016-02-01

    Full Text Available Most common prostaglandin analogs, bimatoprost, latanoprost and travoprost, are licensed for the reduction of elevated intraocular pressure in patients with open angle glaucoma and ocular hypertension, but their non approved use as eyelash enhancers is becoming popular, especially in patients with eyelashes hypotrichosis. A fast and sensitive high performance liquid chromatography tandem mass spectrometry method was developed for the measurement of bimatoprost, latanoprost and travoprost in cosmetic serums freely web-sold to increase eyelash length, thickness and darkness. The analytes and the internal standard (reserpine were separated by reversed phase chromatography with 5 mM ammonium acetate with 0.02% formic acid (mobile phase A and 5 mM ammonium acetate in acetonitrile/water (95/5; v/v with 0.02% formic acid (mobile phase B by gradient elution and detected with tandem mass spectrometry operated in multiple reaction monitoring mode. Linearity between 1 and 500 μg/g shows good correlation coefficients (r2 = 0.99 for all substances. Analytical recovery of analytes under investigation were always higher than 90% and intra-assay and inter-assay precision and accuracy always better than 11%. This method was successfully applied to analyze cosmetic serums freely sold on the Internet websites.

  11. Determination of benzoxazinone derivatives in plants by combining pressurized liquid extraction-solid-phase extraction followed by liquid chromatography-electrospray mass spectrometry.

    Science.gov (United States)

    Villagrasa, Marta; Guillamón, Miriam; Eljarrat, Ethel; Barceló, Damià

    2006-02-22

    A new analytical method based on the use of pressurized liquid extraction (PLE) followed by solid-phase extraction with LiChrolut RP C18 cartridges was evaluated for the sample preparation, extraction, and cleanup of eight naturally occurring benzoxazinone derivatives, 2-beta-D-glucopyranosyloxy-4-hydroxy-1,4-benzoxazin-3-one, 2-beta-D-glucopyranosyloxy-4-hydroxy-7-methoxy-1,4-benzoxazin-3-one, 2,4-dihydroxy-1,4-benzoxazin-3-one (DIBOA), 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one, 2-hydroxy-1,4-benzoxazin-3-one, 2-hydroxy-7-methoxy-1,4-benzoxazin-3-one, benzoxazolin-2-one, and 6-methoxybenzoxazolin-2-one in plant samples. Afterward, liquid chromatography-electrospray mass spectrometry, using the selected ion monitoring mode and internal standard (2-MeO-DIBOA, indoxyl-beta-D-glucoside, and quercetin-3-O-rutinoside) quantification method was performed. This paper demonstrates the effectiveness of the PLE method, in conjunction with sensitive and specific mass spectrometric detection, for the quantitative recovery of compounds of the benzoxazinone class from plants. The recoveries of the analytes ranged from 66 to 110% with coefficients of variation ranging from 1 to 14%. This method gave detection limits between 1 and 27 microg/g. The method was applied to foliage and roots of three different wheat cultivars, and the analytes were detected in the range of 11-3261 microg/g of dry weight.

  12. Analysis of endocrine disruptor compounds in marine sediments by in cell clean up-pressurized liquid extraction-liquid chromatography tandem mass spectrometry determination.

    Science.gov (United States)

    Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

    2014-12-10

    A less time-, solvent- and sorbent-consuming analytical methodology for the determination of bisphenol A and alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) in marine sediment was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The SPLE extraction conditions were optimized by a Plackett-Burman design followed by a central composite design. Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 94 and 100% and repeatability and intermediate precision were <6% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.17 (4-n-nonylphenol) and 4.01 ng g(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of this green methodology. As an application, marine sediment samples from Galicia coast (NW of Spain) were analysed. Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 20.1 and 1409 ng g(-1) dry weight, respectively. Sediment toxicity was estimated and no risk to aquatic biota was found.

  13. Sampling frequency, response times and embedded signal filtration in fast, high efficiency liquid chromatography: A tutorial.

    Science.gov (United States)

    Wahab, M Farooq; Dasgupta, Purnendu K; Kadjo, Akinde F; Armstrong, Daniel W

    2016-02-11

    With increasingly efficient columns, eluite peaks are increasingly narrower. To take full advantage of this, choice of the detector response time and the data acquisition rate a.k.a. detector sampling frequency, have become increasingly important. In this work, we revisit the concept of data sampling from the theorem variously attributed to Whittaker, Nyquist, Kotelnikov, and Shannon. Focusing on time scales relevant to the current practice of high performance liquid chromatography (HPLC) and optical absorbance detection (the most commonly used method), even for very narrow simulated peaks Fourier transformation shows that theoretical minimum sampling frequency is still relatively low (fast chromatography on a state-of-the-art column (38,000 plates), we evaluate the responses produced by different present generation instruments, each with their unique black box digital filters. We show that the common wisdom of sampling 20 points per peak can be inadequate for high efficiency columns and that the sampling frequency and response choices do affect the peak shape. If the sampling frequency is too low or response time is too large, the observed peak shapes will not remain as narrow as they really are - this is especially true for high efficiency and high speed separations. It is shown that both sampling frequency and digital filtering affect the retention time, noise amplitude, peak shape and width in a complex fashion. We show how a square-wave driven light emitting diode source can reveal the nature of the embedded filter. We discuss time uncertainties related to the choice of sampling frequency. Finally, we suggest steps to obtain optimum results from a given system.

  14. Flavonoid profiling of a traditional Chinese medicine formula of Huangqin Tang using high performance liquid chromatography

    Science.gov (United States)

    Li, Tao; Zhuang, Shuaixing; Wang, Yiwei; Wang, Yanli; Wang, Weihao; Zhang, Huihui; Chen, Li; Wang, Dunfang; Zhou, Zhongming; Yang, Weipeng

    2016-01-01

    The quality control processes for herbal medicines have been problematic. Flavonoids are the major active components of Huangqin Tang (HQT, a traditional Chinese medicine formula). In this study, we used a combinative method approach consisting of chromatographic fingerprinting (high performance liquid chromatography; HPLC), quantitative methods and a pharmacodynamic evaluation model to analyze the flavonoids of HQT obtained from different sources. Ten batches of HQT were analyzed by the HPLC fingerprinting method and 26 common peaks were detected, of which 23 peaks corresponded with the chemical profile of HQT. In addition, 11 major compounds were identified by LC–MS analysis (liquid chromatography–tandem mass spectrometer; LC–MSn) and quantified by the HPLC quantitative method approach. The studied 10 batches of HQT were found to be homogeneous in their composition with a similarity between 0.990 and 1.000. The distribution of the 11 identified compounds was found to be very similar among the batches. Only slight pharmacodynamic differences were detected between the different batches, confirming the homogeneity of HQT. The results of this study prove that the combination of chromatographic fingerprinting and quantitative analysis can be readily used for comprehensive quality control of herbal medicines. PMID:27006899

  15. [Measurement of 11 benzophenone ultraviolet-filters in cosmetics by high performance liquid chromatography].

    Science.gov (United States)

    Qu, Baocheng; Bian, Haitao; Mao, Xiqin; Li, Jin

    2015-12-01

    A sample preparation and analytical method with liquid-liquid extraction (LLE) and high performance liquid chromatography (HPLC) was developed to detect 11 benzophenone ultraviolet-filters in cosmetics. The target compounds were extracted by the mixed solutions of tetrahydrofuran (TH)/methanol/water or dichloromethane/water at proper ratios. The extracts were centrifuged and filtered to remove matrix compounds, and then analyzed by HPLC. The separation of analytes was carried out on a Diamonsil-C18 column (150 mm x 4.6 mm, 5 μm) with 0.1% (v/v) formic acid aqueous solution (containing 10 mmol/L ammonium acetate) as mobile phase A and methanol containing 0.1% (v/v) formic acid as mobile phase B. The spiked recoveries of the method (n = 7) were 93.4%-103.8% with the relative standard deviations of 0.1%-4.2%. The limits of detection (LODs) were in the range of 4.0-30 μg/g and the limits of quantitation (LOQs) ranged from 15 to 100 μg/g. The method was applied to the determination of 42 cosmetic samples randomly purchased from the supermarket in Dalian. Five benzophenone series were always detected, in which the content of benzophenone-3 in sunscreen cream and the content of benzophenone-2 in perfume were very high and reached 2 785 μg/g and 2 106 μg/g, respectively. The results showed that the developed method is efficient, reliable and sensitive, which can be applied to the determination of benzophenones in cosmetics.

  16. Determination of eight fluoroquinolones in groundwater samples with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction prior to high-performance liquid chromatography and fluorescence detection.

    Science.gov (United States)

    Vázquez, M M Parrilla; Vázquez, P Parrilla; Galera, M Martínez; García, M D Gil

    2012-10-20

    An ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (US-IL-DLLME) procedure was developed for the extraction of eight fluoroquinolones (marbofloxacin, norfloxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, oxolinic acid and nalidixic acid) in groundwater, using high-performance liquid chromatography with fluorescence detection (HPLC-FD). The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution using a small volume of disperser solvent (0.4 mL of methanol), which increased the extraction efficiency and reduced the equilibrium time. For the DLLME procedure, the IL 1-octyl-3-methylimidazolium hexafluorophosphate ([C(8)MIM] [PF(6)]) and methanol (MeOH) were used as extraction and disperser solvent, respectively. By comparing [C(8)MIM] [PF(6)] with 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM] [PF(6)]) and 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)MIM] [PF(6)]) as extraction solvents, it was observed that when using [C(8)MIM] [PF(6)] the cloudy solution was formed more readily than when using [C(6)MIM] [PF(6)] or [C(4)MIM] [PF(6)]. The factors affecting the extraction efficiency, such as the type and volume of ionic liquid, type and volume of disperser solvent, cooling in ice-water, sonication time, centrifuging time, sample pH and ionic strength, were optimised. A slight increase in the recoveries of fluoroquinolones was observed when an ice-water bath extraction step was included in the analytical procedure (85-107%) compared to those obtained without this step (83-96%). Under the optimum conditions, linearity of the method was observed over the range 10-300 ng L(-1) with correlation coefficient >0.9981. The proposed method has been found to have excellent sensitivity with limit of detection between 0.8 and 13 ng L(-1) and precision with relative standard deviation values between 4.8 and 9.4% (RSD, n=5). Good enrichment factors (122-205) and recoveries (85

  17. A single-step pesticide extraction and clean-up multi-residue analytical method by selective pressurized liquid extraction followed by on-line solid phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for complex matrices.

    Science.gov (United States)

    Rodrigues, Elsa Teresa; Pardal, Miguel Ângelo; Salgueiro-González, Noelia; Muniategui-Lorenzo, Soledad; Alpendurada, Maria Fátima

    2016-06-24

    Pesticides, a group of compounds linked to human activity, may, when in toxic levels, have a profound effect on water quality, and hence result in adverse consequences to aquatic life and ultimately to human health. Analytical challenges arise when successfully trying to determine these levels in environmental complex matrices. Therefore, fast, simple, sensitive and selective analytical methodologies for multi-residue determination of pesticides (atrazine, azoxystrobin, bentazon, λ-cyhalothrin, penoxsulam and terbuthylazine) in sediment, macrophytes (algae and aquatic plants) and aquatic animals were developed and validated. The established methods were matrix-dependent and were based on Selective Pressurized Liquid Extraction (SPLE) followed by on-line Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (on-line SPE-UPLC-ESI-MS/MS). This cutting-edge research methodology uses a small amount of sample, is time saving and reduces the use of organic solvents in compliance with Green Chemistry principles. The analytical features were adequate for all compounds in all studied matrices. The established methodology was applied on real marine samples and no pesticide concentrations above their respective method quantification limits were measured in sediments or aquatic plants. However, terbuthylazine was found in the macroalgae Ulva spp. (108ngg(-1)dw) and all the prospected pesticides were measured above their respective method quantification limits in the bivalve Scrobicularia plana (atrazine: 48ngg(-1)dw, azoxystrobin: 64ngg(-1)dw, bentazon: 33ngg(-1)dw, λ-cyhalothrin: 2531ngg(-1)dw, penoxsulam: 50ngg(-1)dw, and terbuthylazine: 44ngg(-1)dw).

  18. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  19. 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 ...

  20. Analysis of native human plasma proteins and haemoglobin for the presence of bityrosine by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Daneshvar, B; Frandsen, H; Dragsted, L O

    1997-01-01

    fluorescent substance, bityrosine. High-performance liquid chromatography (HPLC) analysis of acid hydrolyzed serum albumin after oxidation with peroxidase/H2O2 or with Cu++/H2O2 showed that bityrosine had been formed whereas oxidation of this protein with Fe(III)/ascorbate did not result in the formation...

  1. The Determination of Polyethylene Glycol in Untreated Urine Samples by High Performance Liquid Chromatography for Intestinal Permeability Studies

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Pedersen, Walther Batsberg; Philipsen, E.

    1985-01-01

    Polyethylene glycol in urine samples has been investigated by high performance liquid chromatography. The molecular weights ranged from 634 to 1338. The urine samples were applied to the chromatographic system without any pre-treatment. For samples with a concentration of 0.2% polyethylene glycol...

  2. Constructing a LabVIEW-Controlled High-Performance Liquid Chromatography (HPLC) System: An Undergraduate Instrumental Methods Exercise

    Science.gov (United States)

    Smith, Eugene T.; Hill, Marc

    2011-01-01

    In this laboratory exercise, students develop a LabVIEW-controlled high-performance liquid chromatography system utilizing a data acquisition device, two pumps, a detector, and fraction collector. The programming experience involves a variety of methods for interface communication, including serial control, analog-to-digital conversion, and…

  3. Using reversed phase high performance liquid chromatography to study the complexation of anthocyanins with β-cyclodextrin

    Science.gov (United States)

    Deineka, V. I.; Lapshova, M. S.; Deineka, L. A.

    2014-06-01

    It is shown by means of reversed phase high performance liquid chromatography (RP HPLC) with mobile phases containing additions of β-cyclodextrin that 5-glucosides of cyanidin and pelargonidin form stronger inclusion complexes than 3-glucosides; this is explained by the steric interference of the glucoside radical.

  4. Elucidation and identification of amino acid containing membrane lipids using liquid chromatography/high-resolution mass spectrometry

    NARCIS (Netherlands)

    Moore, E.K.; Hopmans, E.C.; Rijpstra, W.I.C.; Villanueva, L.; Sinninghe Damsté, J.S.

    2016-01-01

    RATIONALE: Intact polar lipids (IPLs) are the building blocks of cell membranes, and amino acid containing IPLs havebeen observed to be involved in response to changing environmental conditions in various species of bacteri a. High-performance liquid chromatography/mass spectrometry (HPLC/MS) has be

  5. NONLINEAR-REGRESSION METHODS FOR MODELING OF HETEROSCEDASTIC RETENTION DATA IN REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    HENDRIKS, MMWB; COENEGRACHT, PMJ; DOORNBOS, DA

    1994-01-01

    New models have been developed that accurately describe the response surfaces of capacity factors that are a function of changes in the pH and the fraction of organic modifier in reversed-phase high-performance liquid chromatography (RP-HPLC). The purpose of this article is to illustrate one of the

  6. 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…

  7. Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2016-04-01

    In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures.

  8. Evaluation of gardenia yellow using crocetin from alkaline hydrolysis based on ultra high performance liquid chromatography and high-speed countercurrent chromatography.

    Science.gov (United States)

    Inoue, Koichi; Tanada, Chihiro; Nishikawa, Hiroaki; Matsuda, Satoru; Tada, Atsuko; Ito, Yusai; Min, Jun Zhe; Todoroki, Kenichiro; Sugimoto, Naoki; Toyo'oka, Toshimasa; Akiyama, Hiroshi

    2014-12-01

    Gardenia yellow is globally the most valuable spice and food color. It is generally a mixture of water-soluble carotenoid glycosyl esters which consist of crocetin bis(gentiobiosyl) ester as the main component. Crocetin is a natural carotenoid dicarboxylic acid that may be a candidate drug for pharmaceutical development, however, it is either present in trace amounts or is absent in natural gardenia yellow products. We here propose that crocetin produced by alkaline hydrolysis can be used to qualitatively evaluate gardenia yellow products using an ultra high performance liquid chromatographic assay. A useful and efficient isolation technique for isolating high-purity crocetin from gardenia yellow using high-speed countercurrent chromatography is described. High-speed countercurrent chromatographic fractionation followed by an ultra high performance liquid chromatographic assay showed that trans-crocetin is easily converted to about 15% cis-crocetin (85% trans-crocetin). Crocetin in gardenia yellow was quantitatively evaluated. Our approach is based on the hydrolysis process for converting crocetin glycosyl esters to crocetin before evaluation and isolation using the ultra high performance liquid chromatographic and high-speed countercurrent chromatographic methods. The combination of hydrolysis and chromatographic methods allows evaluation of the purity and quantity of crocetin in gardenia yellow.

  9. A field survey of metal binding to metallothionein and other cytosolic ligands in liver of eels using an on-line isotope dilution method in combination with size exclusion (SE) high pressure liquid chromatography (HPLC) coupled to Inductively Coupled Plasma time-of-flight Mass Spectrometry (ICP-TOFMS).

    Science.gov (United States)

    Van Campenhout, Karen; Goenaga Infante, Heidi; Goemans, Geert; Belpaire, Claude; Adams, Freddy; Blust, Ronny; Bervoets, Lieven

    2008-05-15

    The effect of metal exposure on the accumulation and cytosolic speciation of metals in livers of wild populations of European eel with special emphasis on metallothioneins (MT) was studied. Four sampling sites in Flanders showing different degrees of heavy metal contamination were selected for this purpose. An on-line isotope dilution method in combination with size exclusion (SE) high pressure liquid chromatography (HPLC) coupled to Inductively Coupled Plasma time-of-flight Mass Spectrometry (ICP-TOFMS) was used to study the cytosolic speciation of the metals. The distribution of the metals Cd, Cu, Ni, Pb and Zn among cytosolic fractions displayed strong differences. The cytosolic concentration of Cd, Ni and Pb increased proportionally with the total liver levels. However, the cytosolic concentrations of Cu and Zn only increased above a certain liver tissue threshold level. Cd, Cu and Zn, but not Pb and Ni, were largely associated with the MT pool in correspondence with the environmental exposure and liver tissue concentrations. Most of the Pb and Ni and a considerable fraction of Cu and Zn, but not Cd, were associated to High Molecular Weight (HMW) fractions. The relative importance of the Cu and Zn in the HMW fraction decreased with increasing contamination levels while the MT pool became progressively more important. The close relationship between the cytosolic metal load and the total MT levels or the metals bound on the MT pool indicates that the metals, rather than other stress factors, are the major factor determining MT induction.

  10. Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

    Science.gov (United States)

    Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

    2015-06-01

    A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples.

  11. Quality Evaluation of Potentilla fruticosa L. by High Performance Liquid Chromatography Fingerprinting Associated with Chemometric Methods

    Science.gov (United States)

    Liu, Wei; Wang, Dongmei; Liu, Jianjun; Li, Dengwu; Yin, Dongxue

    2016-01-01

    The present study was performed to assess the quality of Potentilla fruticosa L. sampled from distinct regions of China using high performance liquid chromatography (HPLC) fingerprinting coupled with a suite of chemometric methods. For this quantitative analysis, the main active phytochemical compositions and the antioxidant activity in P. fruticosa were also investigated. Considering the high percentages and antioxidant activities of phytochemicals, P. fruticosa samples from Kangding, Sichuan were selected as the most valuable raw materials. Similarity analysis (SA) of HPLC fingerprints, hierarchical cluster analysis (HCA), principle component analysis (PCA), and discriminant analysis (DA) were further employed to provide accurate classification and quality estimates of P. fruticosa. Two principal components (PCs) were collected by PCA. PC1 separated samples from Kangding, Sichuan, capturing 57.64% of the variance, whereas PC2 contributed to further separation, capturing 18.97% of the variance. Two kinds of discriminant functions with a 100% discrimination ratio were constructed. The results strongly supported the conclusion that the eight samples from different regions were clustered into three major groups, corresponding with their morphological classification, for which HPLC analysis confirmed the considerable variation in phytochemical compositions and that P. fruticosa samples from Kangding, Sichuan were of high quality. The results of SA, HCA, PCA, and DA were in agreement and performed well for the quality assessment of P. fruticosa. Consequently, HPLC fingerprinting coupled with chemometric techniques provides a highly flexible and reliable method for the quality evaluation of traditional Chinese medicines. PMID:26890416

  12. Quality Evaluation of Potentilla fruticosa L. by High Performance Liquid Chromatography Fingerprinting Associated with Chemometric Methods.

    Directory of Open Access Journals (Sweden)

    Wei Liu

    Full Text Available The present study was performed to assess the quality of Potentilla fruticosa L. sampled from distinct regions of China using high performance liquid chromatography (HPLC fingerprinting coupled with a suite of chemometric methods. For this quantitative analysis, the main active phytochemical compositions and the antioxidant activity in P. fruticosa were also investigated. Considering the high percentages and antioxidant activities of phytochemicals, P. fruticosa samples from Kangding, Sichuan were selected as the most valuable raw materials. Similarity analysis (SA of HPLC fingerprints, hierarchical cluster analysis (HCA, principle component analysis (PCA, and discriminant analysis (DA were further employed to provide accurate classification and quality estimates of P. fruticosa. Two principal components (PCs were collected by PCA. PC1 separated samples from Kangding, Sichuan, capturing 57.64% of the variance, whereas PC2 contributed to further separation, capturing 18.97% of the variance. Two kinds of discriminant functions with a 100% discrimination ratio were constructed. The results strongly supported the conclusion that the eight samples from different regions were clustered into three major groups, corresponding with their morphological classification, for which HPLC analysis confirmed the considerable variation in phytochemical compositions and that P. fruticosa samples from Kangding, Sichuan were of high quality. The results of SA, HCA, PCA, and DA were in agreement and performed well for the quality assessment of P. fruticosa. Consequently, HPLC fingerprinting coupled with chemometric techniques provides a highly flexible and reliable method for the quality evaluation of traditional Chinese medicines.

  13. On-line high speed lipid extraction for nanoflow liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lee, Ju Yong; Yang, Joon Seon; Park, Se Mi; Byeon, Seul Kee; Moon, Myeong Hee

    2016-09-16

    An on-line lipid extraction method is introduced by utilizing a short capillary extraction column using HILIC and C4 particles prior to nanoflow liquid chromatography-tandem mass spectrometry (nLC-MS/MS). The on-line extraction using a urine sample spiked with PL standards showed similar or slightly higher recovery values (86%-96%) of phospholipids (PLs) compared to those obtained by the conventional off-line extraction based on the Folch method with or without using the air-exposed drying process. In this study, we demonstrated that PL oxidation can occur during the air-exposed drying process of lipid extracts in standard liquid-liquid extraction procedures, which was confirmed by the oxidized PL (OxPL) molecules that were generated from an off-line extraction using a few PL standards. Quantitative comparison of these OxPL species between on- and off-line extraction followed by nLC-MS/MS with multiple reaction monitoring (MRM) analysis showed a significant decrease (2-10 fold) in unwanted OxPL species when on-line extraction was employed. While the number of identified PLs from a urine sample was somewhat lower than those by off-line extraction, the number of OxPLs was significantly reduced (from 70 to 22) with on-line extraction. The new method offers high speed (∼5min) automated extraction of PLs with nLC-MS/MS analysis and presents the possibility of handling a biological sample with a very limited amount of lipids.

  14. Suitability of selective pressurized liquid extraction combined with gas chromatography-ion-trap tandem mass spectrometry for the analysis of polybrominated diphenyl ethers.

    Science.gov (United States)

    Losada, S; Parera, J; Abalos, M; Abad, E; Santos, F J; Galceran, M T

    2010-09-23

    A one-step extraction and clean-up method using pressurized liquid extraction (PLE) (selective PLE) combined with gas chromatography-ion-trap tandem mass spectrometry (GC-ITMS-MS) was evaluated for the analysis of polybrominated diphenyl ethers (from tri- to hepta-PBDEs) at low concentrations in fish and shellfish samples. To this end, the performance of an on-line PLE extraction/clean-up method and of a classical Soxhlet extraction and clean-up method using a multi-layer modified silica column were compared. The two sample treatment methods provided similar results, although an important reduction in the sample treatment time (40 min per sample) was achieved using the selective PLE method. In addition, the suitability of the PLE combined with GC-ITMS-MS method was evaluated by comparing the results obtained in the analysis of fish samples with those obtained by gas chromatography-high resolution mass spectrometry (GC-HRMS). Good agreement between both techniques was obtained with differences between the mean values of less than 16%. The selective PLE method coupled to GC-ITMS-MS produced accurate results for PBDE determination with low limits of detection (1.0-16.8 pg g(-1) wet weight) and quantification (3.1-51 pg g(-1) wet weight) as well as good precision (RSD<16%). This method has been applied to the analysis of PBDEs in fish and shellfish samples collected at fish markets in Catalonia (NE Spain).

  15. Monitoring gradient profile on-line in micro- and nano-high performance liquid chromatography using conductivity detection.

    Science.gov (United States)

    Zhang, Min; Chen, Apeng; Lu, Joann J; Cao, Chengxi; Liu, Shaorong

    2016-08-19

    In micro- or nano-flow high performance liquid chromatography (HPLC), flow-splitters and gradient elutions are commonly used for reverse phase HPLC separations. When a flow splitter was used at a high split-ratio (e.g., 1000:1 or higher), the actual gradient may deviate away from the programmed gradient. Sometimes, mobile phase concentrations can deviate by as much as 5%. In this work, we noticed that the conductivity (σ) of a gradient decreased with the increasing organic-solvent fraction (φ). Based on the relationship between σ and φ, a method was developed for monitoring gradient profile on-line to record any deviations in these HPLC systems. The conductivity could be measured by a traditional conductivity detector or a capacitively coupled contactless conductivity detector (C(4)D). The method was applied for assessing the performance of an electroosmotic pump (EOP) based nano-HPLC. We also observed that σ value of the gradient changed with system pressure; a=0.0175ΔP (R(2)=0.964), where a is the percentage of the conductivity increase and ΔP is the system pressure in bar. This effect was also investigated.

  16. High-pressure liquid chromatographic separation of the naturally occurring toxicants myristicin, related aromatic ethers and falcarinol.

    Science.gov (United States)

    Wulf, L W; Nagel, C W; Branen, A L

    1978-11-21

    The naturally occurring toxicants myristicin, twelve related aromatic ethers and the toxic acetylenic alcohol, falcarinol, were separated from one another by high-pressure liquid chromatography (HPLC). The technique employed a microparticulate nitrile phase column and used heptane and tetrahydrofuran as the eluting solvents. Preparative HPLC with 5-micrometer silica allowed isolation of gram quantities of parsleyapiole and dillapiole from extracts of plain parsley seeds and dill seeds, respectively. Commercially available myristicin as well as other aromatic ethers were also purified in gram quantities with the preparative column.

  17. High pressure liquid chromatographic analysis of the main pungent principles of solar dried West Indian ginger (Zingiber officinale Roscoe)

    Energy Technology Data Exchange (ETDEWEB)

    Balladin, D.A.; Headley, O. [University of the West Indies, Cave Hill Campus, St. Michael, Barbados (West Indies). Centre for Resource Management and Environmental Studies; Chang-Yen, I. [University of the West Indies, St. Augustine Campus, Trinidad (West Indies). Faculty of Agriculture and Natural Sciences; McGaw, D.R. [University of the West Indies, St. Augustine Campus, Trinidad (West Indies). Dept. of Chemical Engineering

    1998-12-31

    The main pungent principles of West Indian ginger (Zingiber officinale Roscoe) were quantified and qualified using High Pressure Liquid Chromatography. This procedure was used to evaluate the pungency profile of fresh, solar dried and solar dried/steam distilled ginger rhizomes. In this investigation, the total oleoresin extracted was in the ratio [20: 1: 2] for [fresh ginger: solar dried: solar dried/steam distilled ginger rhizomes] with respect to the [6]-gingerol content. This simple isocratic HPLC method can be used to investigate the pungency profile of the extracted oleoresin from the ginger rhizomes. (author)

  18. Screening antiallergic components from Carthamus tinctorius using rat basophilic leukemia 2H3 cell membrane chromatography combined with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Han, Shengli; Huang, Jing; Cui, Ronghua; Zhang, Tao

    2015-02-01

    Carthamus tinctorius, used in traditional Chinese medicine, has many pharmacological effects, such as anticoagulant effects, antioxidant effects, antiaging effects, regulation of gene expression, and antitumor effects. However, there is no report on the antiallergic effects of the components in C. tinctorius. In the present study, we investigated the antiallergic components of C. tinctorius and its mechanism of action. A rat basophilic leukemia 2H3/cell membrane chromatography coupled online with high-performance liquid chromatography and tandem mass spectrometry method was developed to screen antiallergic components from C. tinctorius. The screening results showed that Hydroxysafflor yellow A, from C. tinctorius, was the targeted component that retained on the rat basophilic leukemia 2H3/cell membrane chromatography column. We measured the amount of β-hexosaminidase and histamine released in mast cells and the key markers of degranulation. The release assays showed that Hydroxysafflor yellow A could attenuate the immunoglobulin E induced release of allergic cytokines without affecting cell viability from 1.0 to 50.0 μM. In conclusion, the established rat basophilic leukemia 2H3 cell membrane chromatography coupled with online high-performance liquid chromatography and tandem mass spectrometry method successfully screened and identified Hydroxysafflor yellow A from C. tinctorius as a potential antiallergic component. Pharmacological analysis elucidated that Hydroxysafflor yellow A is an effective natural component for inhibiting immunoglobulin E-antigen-mediated degranulation.

  19. Quantitative Analysis of Sphingomyelin by High-Performance Liquid Chromatography after Enzymatic Hydrolysis

    Directory of Open Access Journals (Sweden)

    Seunghyun Lee

    2012-01-01

    Full Text Available Sphingomyelin is the most abundant sphingolipid in mammalian cells and is mostly present in the plasma membrane. A new analytical method using high-performance liquid chromatography (HPLC was developed to quantify sphingomyelin in mouse plasma and tissues, 3T3-L1 cells, rat aortic smooth muscle cells, and HT-29 cells. Sphingomyelin and dihydrosphingomyelin, an internal standard, were separated by high-performance thin-layer chromatography and simultaneously hydrolyzed with sphingolipid ceramide N-deacylase and sphingomyelinase to release sphingosine and dihydrosphingosine, respectively. Sphingomyelin content was measured by HPLC following o-phthalaldehyde derivatization. Sphingomyelin concentrations in 3T3-L1 cells, rat aortic smooth muscle cells, and HT-29 cells were 60.10±0.24, 62.69±0.08, and 58.38±0.37 pmol/μg protein, respectively, whereas those in brain, kidney, and liver of ICR mice were 55.60±0.43, 43.75±0.21, and 22.26±0.14 pmol/μg protein. The sphingomyelin concentration in mouse plasma was 407.40±0.31 μM. The limits of detection and quantification for sphingomyelin were 5 and 20 pmol, respectively, in the HPLC analysis with fluorescence detection. This sensitivity was sufficient for analyzing sphingomyelin in biological samples. In conclusion, this analytical method is a sensitive and specific technique for quantifying sphingomyelin and was successfully applied to diverse biological samples with excellent reproducibility.

  20. Determination of multiple phytohormones in fruits by high-performance liquid chromatography with fluorescence detection using dispersive liquid-liquid microextraction followed by precolumn fluorescent labeling.

    Science.gov (United States)

    Li, Guoliang; Lu, Shuaimin; Wu, Hongliang; Chen, Guang; Liu, Shucheng; Kong, Xiaojian; Kong, Weiheng; You, Jinmao

    2015-01-01

    Plant hormone determination in food matrices has attracted more and more attention because of their potential risks to human health. However, analytical methods for the analysis of multiple plant hormones remain poorly investigated. In the present study, a convenient, selective, and ultrasensitive high-performance liquid chromatography method for the simultaneous determination of multiple classes of plant hormones has been developed successfully using dispersive liquid-liquid microextraction followed by precolumn fluorescent labeling. Eight plant hormones in fruits including jasmonic acid, 12-oxo-phytodienoic acid, indole-3-acetic acid, 3-indolybutyric acid, 3-indolepropionic acid, gibberellin A3 , 1-naphthylacetic acid, and 2-naphthaleneacetic acid were analyzed by this method. The conditions employed for dispersive liquid-liquid microextraction were optimized systematically. The linearity for all plant hormones was found to be >0.9993 (R(2) values). This method offered low detection limits of 0.19-0.44 ng/mL (at a signal-to-noise ratio of 3), and method accuracies were in the range of 92.32-103.10%. The proposed method was applied to determine plant hormones in five kinds of food samples, and this method can achieve a short analysis time, low threshold levels of detection, and a high specificity for the analysis of targeted plant hormones present at trace level concentrations in complex matrices.

  1. Enantiomeric separation of organophosphorus pesticides by high-performance liquid chromatography, gas chromatography and capillary electrophoresis and their applications to environmental fate and toxicity assays.

    Science.gov (United States)

    Li, Ling; Zhou, Shanshan; Jin, Lixia; Zhang, Cheng; Liu, Weiping

    2010-05-15

    In recent years, the continuous evolution of the field of stereochemistry has produced a heightened awareness of the applications of pure enantiomers of agrochemicals. This review describes reports of the enantiomeric separation of commercial organophosphorus pesticides (OPs) and the applications of these methods to research on the enantioselectivity of the toxicity and environmental fate of these compounds. Chiral OPs can be analysed by high-performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE). These different separation techniques for OP enantiomers are briefly discussed, and their applications are presented.

  2. Sequence-dpenedent DNA separation by anion-exchange high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yamakawa, Hisashi; Higashino, Ken-ich; Ohara, Osamu [Kazusa DNA Research Inst., Chiba (Japan)

    1996-09-05

    High-performance liquid chromatography (HPLC) system with a new nonporous anion-exchange resin, DNA-NPR, made it possible to rapidly separate DNA fragments up to 20 kbp with high resolution. In order to further characterize this chromatographic DNA separation system, we prepared a mixtures of double-stranded DNAs of constant length carrying a fully degenerated 50-bp region and analyzed their chromatographic behavior on the DNA-NPR column. The results indicated that the separation of DNA fragments on the anion-exchange HPLC was governed not only by size, but also by nucleotide sequence: even DNA fragments with the same size and the same base content could be separated on this column. Taking advantage of this characteristic feature of the anion-exchange HPLC, we could readily fractionate human cDNAs with practically acceptable recovery and high resolution. Furthermore, the combination of HPLC and gel electrophoresis realized separation of a mixture of DNA fragments in a two-dimensional pattern. 22 refs., 5 figs., 1 tab.

  3. Determination of rare earth elements in high purity rare earth oxides by liquid chromatography, thermionic mass spectrometry and combined liquid chromatography/thermionic mass spectrometry

    Science.gov (United States)

    Stijfhoorn, D. E.; Stray, H.; Hjelmseth, H.

    1993-03-01

    A high-performance liquid Chromatographie (HPLC) method for the determination of rare earth elements in rocks has been modified and used for the determination of rare earth elements (REE) in high purity rare earth oxides. The detection limit was 1-1.5 ng or 2-3 mg/kg when a solution corresponding to 0.5 mg of the rare earth oxide was injected. The REE determination was also carried out by adding a mixture of selected REE isotopes to the sample and analysing the collected HPLC-fractions by mass spectrometry (MS) using a thermionic source. Since the matrix element was not collected, interference from this element during the mass spectrometric analysis was avoided. Detection limits as low as 0.5 mg/kg could then be obtained. Detection limits as low as 0.05 mg/kg were possible by MS without HPLC-pre-separation, but this approach could only be used for those elements that were not affected by the matrix. Commercial samples of high purity Nd 2O 3, Gd 2O 3 and Dy 2O 3 were analysed in this study, and a comparison of results obtained by HPLC, combined HPLC/MS and direct MS are presented.

  4. High performance liquid chromatography--atomic fluorescence spectrometric determination of arsenic species in beer samples

    Energy Technology Data Exchange (ETDEWEB)

    Melo Coelho, N.M.; Parrilla, Carmen; Cervera, M.L.; Pastor, A.; Guardia, M. de la

    2003-04-10

    A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation--atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH{sub 2}PO{sub 4}/K{sub 2}HPO{sub 4} as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 {mu}l, a 4.0% (m/v) solution of sodium tetrahydroborate and 2.0 mol l{sup -1} hydrochloric acid with flow rates of 2.7 and 1.7 ml min{sup -1}, respectively and a flow rate of 500 ml min{sup -1} for the argon carrier gas. Under the best experimental conditions, the detection limit was found to be 0.12, 0.20, 0.27 and 0.39 {mu}g l{sup -1} for As(III), DMA, MMA and As(V), respectively. The relative standard deviation for eight independent determinations varied from 3.9 till 8.9% for species considered at a concentration level of 10.0 {mu}g l{sup -1}. Recovery and comparative studies evidenced that the method is suitable for the accurate determination of arsenic species in water and beer samples.

  5. Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

    2014-11-01

    An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened.

  6. Rapid determination of organochlorine pesticides in fish using selective pressurized liquid extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Choi, Minkyu; Lee, In-Seok; Jung, Rae-Hong

    2016-08-15

    A rapid automated extraction and cleanup method using selective pressurized liquid extraction was developed and validated for 14 organochlorine pesticides in fish. The lipid-removal efficiencies achieved by adding alumina, Florisil, acid-treated silica gel, and silica gel to the extraction cell were determined and optimized. In the optimized method, fish (2-3g) was placed above alumina (30 g) in the extraction cell, then the sample was extracted using a 7:3 mixture of hexane and dichloromethane. The method was validated using certified reference materials (NIST SRM 1946 and 1974c), spiked fish, and four lipid-rich fish samples. The mean low- and high-concentration spike recoveries were 91% and 93% with RSDextraction and cleanup procedure, including having a short preparation (cleanup and concentration) time and minimal sample contamination and being able to be automated.

  7. High-performance liquid chromatography using UV detection for the simultaneous quantification of ropivacaine and bupivacaine in human plasma.

    Science.gov (United States)

    Gaudreault, François; Drolet, Pierre; Varin, France

    2009-12-01

    A specific high-performance liquid chromatography assay coupled with UV detection has been developed and validated for the simultaneous determination of ropivacaine and bupivacaine in human plasma. A liquid-liquid back extraction procedure was used to increase specificity, and very good and consistent recoveries were obtained: 93%-95% for ropivacaine and 90%-96% for bupivacaine. The lowest limit of quantification was 4 and 8 ng/mL for ropivacaine and bupivacaine, respectively. The method was sensitive, reproducible (coefficient of variation

  8. Rapid estimation of concentration of aromatic classes in middistillate fuels by high-performance liquid chromatography

    Science.gov (United States)

    Otterson, D. A.; Seng, G. T.

    1985-01-01

    An high performance liquid chromatography (HPLC) method to estimate four aromatic classes in middistillate fuels is presented. Average refractive indices are used in a correlation to obtain the concentrations of each of the aromatic classes from HPLC data. The aromatic class concentrations can be obtained in about 15 min when the concentration of the aromatic group is known. Seven fuels with a wide range of compositions were used to test the method. Relative errors in the concentration of the two major aromatic classes were not over 10 percent. Absolute errors of the minor classes were all less than 0.3 percent. The data show that errors in group-type analyses using sulfuric acid derived standards are greater for fuels containing high concentrations of polycyclic aromatics. Corrections are based on the change in refractive index of the aromatic fraction which can occur when sulfuric acid and the fuel react. These corrections improved both the precision and the accuracy of the group-type results.

  9. High-performance liquid chromatography of quinoidal imminium compounds derived from triphenylmethanes

    Science.gov (United States)

    Abidi, S.L.

    1983-01-01

    A series of eleven p-aminotriphenylmethane dyes have been studied by high-performance liquid chromatography (HPLC). The combined use of HPLC and spectrophotometry permits specific detection of these compounds in the visible range around 600 nm. As the high affinity of the imminium cations for the active sites of the hydrocarbonaceous stationary phase has presented difficulties for reversed-phase HPLC with pure solvents, organic electrolytes were added to the mobile phase to facilitate the elution of the components with improved selectivity, sensitivity (minimum detection limit, 0.1 μg/ml), and peak symmetry. The effects of chromatographic variables on the component retentivity were investigated. Retention times of the dye analytes decreased with increasing concentration of the added ionic reagent and with decreasing number of the hydrophobic alkyl substituents on the nitrogen atom. The influence of pH on the retention parameters appears to parallel that observed previously for cationic quaternary ammonium compounds. Among the acidic reagents employed, naphthalenesulfonic acid yielded the most satisfactory results. The use of binary electrolyte systems invariably improved the chromatographic behavior of the imminium solutes analyzed. Results obtained with two different octadecylsilica columns have been compared.

  10. Quantitative structure-retention relationships of pesticides in reversed-phase high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Aschi, Massimiliano [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); D' Archivio, Angelo Antonio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)]. E-mail: darchivi@univaq.it; Maggi, Maria Anna [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); Mazzeo, Pietro [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); Ruggieri, Fabrizio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)

    2007-01-23

    In this paper, a quantitative structure-retention relationships (QSRR) method is employed to predict the retention behaviour of pesticides in reversed-phase high-performance liquid chromatography (HPLC). A six-parameter nonlinear model is developed by means of a feed-forward artificial neural network (ANN) with back-propagation learning rule. Accurate description of the retention factors of 26 compounds including commonly used insecticides, herbicides and fungicides and some metabolites is successfully achieved. In addition to the acetonitrile content, included to describe composition of the water-acetonitrile mobile phase, the octanol-water partition coefficient (from literature) and four quantum chemical descriptors are considered to account for the effect of solute structure on the retention. These are: the total dipole moment, the mean polarizability, the anisotropy of polarizability and a descriptor of hydrogen bonding ability based on the atomic charges on hydrogen bond donor and acceptor chemical functionalities. The proposed nonlinear QSRR model exhibits a high degree of correlation between observed and computed retention factors and a good predictive performance in wide range of mobile phase composition (40-65%, v/v acetonitrile) that supports its application for the prediction of the chromatographic behaviour of unknown pesticides. A multilinear regression model based on the same six descriptors shows a significantly worse predictive capability.

  11. The MAREDAT global database of high performance liquid chromatography marine pigment measurements

    Science.gov (United States)

    Peloquin, J.; Swan, C.; Gruber, N.; Vogt, M.; Claustre, H.; Ras, J.; Uitz, J.; Barlow, R.; Behrenfeld, M.; Bidigare, R.; Dierssen, H.; Ditullio, G.; Fernandez, E.; Gallienne, C.; Gibb, S.; Goericke, R.; Harding, L.; Head, E.; Holligan, P.; Hooker, S.; Karl, D.; Landry, M.; Letelier, R.; Llewellyn, C. A.; Lomas, M.; Lucas, M.; Mannino, A.; Marty, J.-C.; Mitchell, B. G.; Muller-Karger, F.; Nelson, N.; O'Brien, C.; Prezelin, B.; Repeta, D.; Smith, W. O., Jr.; Smythe-Wright, D.; Stumpf, R.; Subramaniam, A.; Suzuki, K.; Trees, C.; Vernet, M.; Wasmund, N.; Wright, S.

    2013-03-01

    A global pigment database consisting of 35 634 pigment suites measured by high performance liquid chromatography was assembled in support of the MARine Ecosytem DATa (MAREDAT) initiative. These data originate from 136 field surveys within the global ocean, were solicited from investigators and databases, compiled, and then quality controlled. Nearly one quarter of the data originates from the Laboratoire d'Océanographie de Villefranche (LOV), with an additional 17% and 19% stemming from the US JGOFS and LTER programs, respectively. The MAREDAT pigment database provides high quality measurements of the major taxonomic pigments including chlorophylls a and b, 19'-butanoyloxyfucoxanthin, 19'-hexanoyloxyfucoxanthin, alloxanthin, divinyl chlorophyll a, fucoxanthin, lutein, peridinin, prasinoxanthin, violaxanthin and zeaxanthin, which may be used in varying combinations to estimate phytoplankton community composition. Quality control measures consisted of flagging samples that had a total chlorophyll a concentration of zero, had fewer than four reported accessory pigments, or exceeded two standard deviations of the log-linear regression of total chlorophyll a with total accessory pigment concentrations. We anticipate the MAREDAT pigment database to be of use in the marine ecology, remote sensing and ecological modeling communities, where it will support model validation and advance our global perspective on marine biodiversity. The original dataset together with quality control flags as well as the gridded MAREDAT pigment data may be downloaded from PANGAEA: http://doi.pangaea.de/10.1594/PANGAEA.793246.

  12. High-performance liquid chromatography method validation for determination of tetracycline residues in poultry meat

    Directory of Open Access Journals (Sweden)

    Vikas Gupta

    2014-01-01

    Full Text Available Background: In this study, a method for determination of tetracycline (TC residues in poultry with the help of high-performance liquid chromatography technique was validated. Materials and Methods: The principle step involved in ultrasonic-assisted extraction of TCs from poultry samples by 2 ml of 20% trichloroacetic acid and phosphate buffer (pH 4, which gave a clearer supernatant and high recovery, followed by centrifugation and purification by using 0.22 μm filter paper. Results: Validity study of the method revealed that all obtained calibration curves showed good linearity (r2 > 0.999 over the range of 40-4500 ng. Sensitivity was found to be 1.54 and 1.80 ng for oxytetracycline (OTC and TC. Accuracy was in the range of 87.94-96.20% and 72.40-79.84% for meat. Precision was lower than 10% in all cases indicating that the method can be used as a validated method. Limit of detection was found to be 4.8 and 5.10 ng for OTC and TC, respectively. The corresponding values of limit of quantitation were 11 and 12 ng. Conclusion: The method reliably identifies and quantifies the selected TC and OTC in the reconstituted poultry meat in the low and sub-nanogram range and can be applied in any laboratory.

  13. Determination of 5-methylcytosine from plant DNA by high-performance liquid chromatography.

    Science.gov (United States)

    Wagner, I; Capesius, I

    1981-06-26

    The relative amounts of the five nucleosides (deoxycytidine, 5-methyldeoxycytidine, deoxyadenosine, deoxyguanosine and thymidine) in the DNA of nine plant species, one plant satellite DNA, and one animal species were determined by high performance liquid chromatography. The method allows the clean separation of the nucleosides from 10 microgram samples with 15 min. The following values for the proportion of methylated cytosines among all cytosines were obtained: Lobularia maritima 18.5%, Nicotiana tabacum 32.6%, Pisum sativum 23.2%, Rhinanthus minor 29.2%, Sinapsis alba 12.2%, Vicia faba 30.5%, Viscum album 23.2%, Cymbidium pumilum 18.8%, Cymbidium pumilum AT-rich satellite DNA 15.8%, Triticum aestivum 22.4%. DNA of an animal, the gerbil, Meriones unguiculatus, had a methylation percentage of 3.1%. An estimate of the GC content based on the buoyant density of DNA tends to be lower than the actual value, an estimate based on the melting temperature tends to be higher. This supports the finding by other authors that DNA methylation decreases the buoyant density and may increase the melting temperature at high m5C concentration.

  14. Determination of Residual Monomers in Polycarboxylate Superplasticizer Using High Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    GUO Liping; WANG Shaofeng; ZHANG Anfu; LEI Jiaheng; DU Xiaodi

    2011-01-01

    A procedure was developed for the determination of residual monomers in polycarboxylate superplasticizer (PCs) by reversed-phase high performance liquid chromatography (RP-HPLC). Four kinds of residual monomers were well separated and determined on a SinoChrom ODS-BP (C18) column with mobile phases composed of acetonitrile and phosphate buffer solution. The monomers were detected by UV detector at 205 nm and quantitatively analyzed with an external standard method. For those residual monomers, the linear response ranged from 4.0× 10-6 mol·L-1 to 2.0× 10-3 mol·L-1. The determination limit of acrylic acid, sodium methylallyl sulfonate and 2-Acrylamido-2-methylpropane sulfonic acid was 0.02× 10-5 mol·L-1, while that of methoxy-polyethylene glycol monoacrylate was 0.1 × 10-5 mol· L-1. The relative standard deviation (RSD) of high concentration samples was less than 1%, while that of the low concentration samples was between 1%-4%. The standard (additional) recovery ratio was 97.4% -104.2%.

  15. Automatic analyzer for highly polar carboxylic acids based on fluorescence derivatization-liquid chromatography.

    Science.gov (United States)

    Todoroki, Kenichiro; Nakano, Tatsuki; Ishii, Yasuhiro; Goto, Kanoko; Tomita, Ryoko; Fujioka, Toshihiro; Min, Jun Zhe; Inoue, Koichi; Toyo'oka, Toshimasa

    2015-03-01

    A sensitive, versatile, and reproducible automatic analyzer for highly polar carboxylic acids based on a fluorescence derivatization-liquid chromatography (LC) method was developed. In this method, carboxylic acids were automatically and fluorescently derivatized with 4-(N,N-dimethylaminosulfonyl)-7-piperazino-2,1,3-benzoxadiazole (DBD-PZ) in the presence of 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride by adopting a pretreatment program installed in an LC autosampler. All of the DBD-PZ-carboxylic acid derivatives were separated on the ODS column within 30 min by gradient elution. The peak of DBD-PZ did not interfere with the separation and the quantification of all the acids with the exception of lactic acid. From the LC-MS/MS analysis, we confirmed that lactic acid was converted to an oxytriazinyl derivative, which was further modified with a dimethoxy triazine group of 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (DMT-MM). We detected this oxytriazinyl derivative to quantify lactic acid. The detection limits (signal-to-noise ratio = 3) for the examined acids ranged from 0.19 to 1.1 µm, which correspond to 95-550 fmol per injection. The intra- and inter-day precisions of typical, highly polar carboxylic acids were all carboxylic acids in various samples, which included fruit juices, red wine and media from cultured tumor cells.

  16. 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.

  17. 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.

  18. Determination of aristolochic acids by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Wang, Yinan; Chan, Wan

    2014-06-25

    Nephrotoxic and carcinogenic aristolochic acids (AAs) are naturally occurring nitrophenanthrene carboxylic acids in the herbal genus Aristolochia. The misuse of AA-containing herbs in preparing slimming drugs has caused hundred of cases of kidney disease in Belgium women in a slimming regime in the early 1990s. Accumulating evidence also suggested that prolong dietary intake of AA-contaminated food is one of the major causes to the Balkan endemic nephropathy that was first observed in the late 1950s. Therefore, analytical methods of high sensitivity are extremely important for safeguarding human exposure to AA-containing herbal medicines, herbal remedies, and food composites. In this paper, we describe the development of a new high-performance liquid chromatography coupled fluorescence detector (HPLC-FLD) method for the sensitive determination of AAs. The method makes use of a novel cysteine-induced denitration reaction that "turns on" the fluorescence of AAs for fluorometric detections. Our results showed that the combination of cysteine-induced denitration and HPLC-FLD analysis allows for sensitive quantification of AA-I and AA-II at detection limits of 27.1 and 25.4 ng/g, respectively. The method was validated and has been successfully applied in quantifying AAs in Chinese herbal medicines.

  19. [Determination of five coumarins in toys by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Yang, Rongjing; Wei, Biwen; Gao, Huan; Yu, Wenjia

    2012-02-01

    A rapid analytical method for the determination of five coumarins (coumarin, 7-methoxycoumarin, dihydrocoumarin, 7-methyl coumarin and 7-ethoxy-4-methyl coumarin) in toys by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed. After ultrasonic extraction in tetrahydrofuran, the samples were analyzed by HPLC-MS/MS in multi-reaction monitoring (MRM) mode. Acetonitrile and 0.1% acetic acid were used as the mobile phases with gradient elution. The linear ranges of calibration curves were 10 - 1 000 microg/L, and the limits of quantification (LOQ) (S/N > 10) were 2.0 microg/L for all the analytes, except that the LOQ for dihydrocoumarin was 5.0 microg/L. The recoveries of the five coumarins spiked in three types of samples were in the ranges of 93.2% - 105.8%, 97.3% - 103.2% and 96.8% - 102.9%, with the relative standard deviations in the ranges of 4.35% - 8.27%, 3.65% - 6.73% and 4.03% - 6.45%, respectively. The method was applied in the determination of 12 toy samples. The five analytes were found in 9 samples, and in some cases, the presence of quite high concentrations of these coumarins in the toys should be a matter of concern.

  20. [Determination of gossypol in edible vegetable oil with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Wenhua; Huang, Chaoqun; Xie, Wen; Shen, Li

    2014-06-01

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of gossypol in edible vegetable oil. The sample was extracted with ethyl alcohol by vortex-excited oscillation. The extract was cleaned up by 0.22 microm filter membrane and centrifuged for 5 min at 4 000 r/min after standing in a fridge at 4 degrees C for 30 min. The compound was separated on a C18 column (100 mm x 2.1 mm, 3.5 microm) with acetonitrile and 1% (v/v) formic acid aqueous solution as mobile phase. The detection of gossypol was carried out by LC-MS/MS with positive electrospray ionization under multiple reaction monitoring (MRM) mode using external standard method. The limits of quantification (S/N > 10) of gossypol in edible vegetable oil was 1 mg/kg. The recoveries were from 87.4% to 100% at the spiked levels of 1, 2, 200 mg/kg of gossypol in edible vegetable oil with the relative standard deviations (RSDs) between 3.9% and 12.2%. The method, with high sensitivity, good precision and high recovery, was suitable for the confirmation and quantification of gossypol residue in edible vegetable oil.

  1. Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

    2017-03-15

    Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL(-1) for the three psychotropic drugs with the correlation of determinations (R(2)s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL(-1) and 1.0-1.5ngmL(-1), respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained.

  2. Quantitation of triacylglycerols in edible oils by off-line comprehensive two-dimensional liquid chromatography-atmospheric pressure chemical ionization mass spectrometry using a single column.

    Science.gov (United States)

    Wei, Fang; Hu, Na; Lv, Xin; Dong, Xu-Yan; Chen, Hong

    2015-07-24

    In this investigation, off-line comprehensive two-dimensional liquid chromatography-atmospheric pressure chemical ionization mass spectrometry using a single column has been applied for the identification and quantification of triacylglycerols in edible oils. A novel mixed-mode phenyl-hexyl chromatographic column was employed in this off-line two-dimensional separation system. The phenyl-hexyl column combined the features of traditional C18 and silver-ion columns, which could provide hydrophobic interactions with triacylglycerols under acetonitrile conditions and can offer π-π interactions with triacylglycerols under methanol conditions. When compared with traditional off-line comprehensive two-dimensional liquid chromatography employing two different chromatographic columns (C18 and silver-ion column) and using elution solvents comprised of two phases (reversed-phase/normal-phase) for triacylglycerols separation, the novel off-line comprehensive two-dimensional liquid chromatography using a single column can be achieved by simply altering the mobile phase between acetonitrile and methanol, which exhibited a much higher selectivity for the separation of triacylglycerols with great efficiency and rapid speed. In addition, an approach based on the use of response factor with atmospheric pressure chemical ionization mass spectrometry has been developed for triacylglycerols quantification. Due to the differences between saturated and unsaturated acyl chains, the use of response factors significantly improves the quantitation of triacylglycerols. This two-dimensional liquid chromatography-mass spectrometry system was successfully applied for the profiling of triacylglycerols in soybean oils, peanut oils and lord oils. A total of 68 triacylglycerols including 40 triacylglycerols in soybean oils, 50 triacylglycerols in peanut oils and 44 triacylglycerols in lord oils have been identified and quantified. The liquid chromatography-mass spectrometry data were analyzed

  3. Multi-detection of corticosteroids in sports doping and veterinary control using high-resolution liquid chromatography/time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Touber, M.E.; Engelen, M.C.; Georgakopoulus, C.; Rhijn, van J.A.; Nielen, M.W.F.

    2007-01-01

    A liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) method was developed using the latest high-resolution LC column technology, the ultra performance liquid chromatography (UPLC (TM)), and electrospray ionization (ESI) in the positive ion mode. Gradient UPLC separation conditions wer

  4. Analysis of the Constituents in “Zhu She Yong Xue Shuan Tong” by Ultra High Performance Liquid Chromatography with Quadrupole Time-of-Flight Mass Spectrometry Combined with Preparative High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Lin-Lin Wang

    2015-11-01

    Full Text Available “Zhu She Yong Xue Shuan Tong” lyophilized powder (ZSYXST, consists of a series of saponins extracted from Panax notoginseng, which has been widely used in China for the treatment of strokes. In this study, an ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS combined with preparative high performance liquid chromatography (PHPLC method was developed to rapidly identify both major and minor saponins in ZSYXST. Some high content components were removed through PHPLC in order to increase the sensitivity of the trace saponins. Then, specific characteristic fragment ions in both positive and negative mode were utilized to determine the types of aglycone, saccharide, as well as the saccharide chain linkages. As a result, 94 saponins, including 20 pairs of isomers and ten new compounds, which could represent higher than 98% components in ZSYXST, were identified or tentatively identified in commercial ZSYXST samples.

  5. Real-Time, Non-Intrusive Detection of Liquid Nitrogen in Liquid Oxygen at High Pressure and High Flow

    Science.gov (United States)

    Singh, Jagdish P.; Yueh, Fang-Yu; Kalluru, Rajamohan R.; Harrison, Louie

    2012-01-01

    An integrated fiber-optic Raman sensor has been designed for real-time, nonintrusive detection of liquid nitrogen in liquid oxygen (LOX) at high pressures and high flow rates in order to monitor the quality of LOX used during rocket engine ground testing. The integrated sensor employs a high-power (3-W) Melles Griot diode-pumped, solid-state (DPSS), frequency-doubled Nd:YAG 532- nm laser; a modified Raman probe that has built-in Raman signal filter optics; two high-resolution spectrometers; and photomultiplier tubes (PMTs) with selected bandpass filters to collect both N2 and O2 Raman signals. The PMT detection units are interfaced with National Instruments Lab- VIEW for fast data acquisition. Studies of sensor performance with different detection systems (i.e., spectrometer and PMT) were carried out. The concentration ratio of N2 and O2 can be inferred by comparing the intensities of the N2 and O2 Raman signals. The final system was fabricated to measure N2 and O2 gas mixtures as well as mixtures of liquid N2 and LOX

  6. Evaluation of aminoacids in irradiated beans (Vigna unguiculata (L.) Walp) by high performance liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Keila S. Cople; Souza, Luciana B.; Coelho, Maysa J.; Lima, Antonio L. Santos; Hernandes, Nilber K. [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil). Secao de Engenharia Nuclear]. E-mail: keila@ime.eb.br; Godoy, Ronoel L.O. [EMBRAPA Agroindustria de Alimentos, Rio de Janeiro, RJ (Brazil)]. E-mail: ronoel@ctaa.embrapa.br

    2007-07-01

    Fradinho-bean (Vigna unguiculata (L.) Walp) is originated from Africa and is known in Brazil as 'caupi', 'corda' or 'macassar'. It is grown in the interior of Northeast Brazil (semi-arid region) and can be found in parts of the North, being one of the most important components of people's diet in those regions. The Northeast area produces around 429,375 ton of fradinho-bean per year. Leguminous plants are very important sources of proteins, vitamins, carbohydrates and minerals. This kind of bean is an excellent source of proteins (around 23- 25% of its nutritional content), being superior to regular beans (Phaseolus vulgaris). The irradiation process is an alternative to avoid post-harvesting losses, without changing the nutritional value of food. This study has the objective to evaluate the effect of different gamma irradiation doses (0.0; 0.5; 1.0; 2.5; 5.0 and 10.0 kGy) on aminoacid content of fradinho-bean by high performance liquid chromatography (HPLC) and the accompanying of the grains during storage time of 6 months. After irradiation, the bean grains went through a milling process in order to make flour for posterior extraction. A liquid chromatographer Waters, model Alliance 2695, with fluorescent detector Waters 2475, having a mobile phase with gradient elution of sodium acetate. acetonitrile and Milli-Q water, was employed. The flux used was 1 mL/min and the injection volume of 10 {mu}L. The column (C 18 150.0 x 3.9 mm) was kept at 36 deg C. The results show that gamma irradiation is a promise process for fradinho bean during conservation storage time of 6 months, until the dose of 10.0 kGy. Even the most radio-sensitive aminoacids like aromatics and basic lateral chains were preserved. (author)

  7. Monosaccharide composition analysis of immunomodulatory polysaccharides by on-line hollow fiber microextraction with high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Nani; Wang, Xuping; Huang, Xiaowen; Mao, Zhujun; Zhang, Yang; Yu, Yong; Shou, Dan

    2016-03-01

    The monosaccharide compositions of functional polysaccharides are essential for structure elucidation and biological activity determination. A sensitive method based on on-line hollow-fiber liquid-phase microextraction with high-performance liquid chromatography has been established for the analysis of ten monosaccharide compositions (two uronic acids, two amino sugars and six neutral sugars) of the immunomodulatory polysaccharides. After derivatization, the sample was injected into the lumen of a hollow fiber immersed in butyl ether and separated by liquid chromatography. Under optimized conditions, the calibration curves were linear (r ≥ 0.9996) in the range of 10-2000 μmol L(-1) . The limits of detection were in the range of 0.04-1.58 μmol L(-1) , and the recoveries were in the range of 92.1-99.6%, which shows that the method is applicable to the analysis of the monosaccharide composition of various polysaccharides.

  8. A dispersive liquid-liquid micellar microextraction for the determination of pharmaceutical compounds in wastewaters using ultra-high-performace liquid chromatography with DAD detection.

    Science.gov (United States)

    Montesdeoca-Esponda, Sarah; Mahugo-Santana, Cristina; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2015-03-01

    A dispersive liquid-liquid micellar microextraction (DLLMME) method coupled with ultra-high-performance liquid chromatography (UHPLC) using Diode Array Detector (DAD) detector was developed for the analysis of five pharmaceutical compounds of different nature in wastewaters. A micellar solution of a surfactant, polidocanol, as extraction solvent (100 μL) and chloroform as dispersive solvent (200 μL) were used to extract and preconcentrate the target analytes. Samples were heated above critical temperature and the cloudy solution was centrifuged. After removing the chloroform, the reduced volume of surfactant was then injected in the UHPLC system. In order to obtain high extraction efficiency, the parameters affecting the liquid-phase microextraction, such as time and temperature extraction, ionic strength and surfactant and organic solvent volume, were optimized using an experimental design. Under the optimized conditions, this procedure allows enrichment factors of up to 47-fold. The detection limit of the method ranged from 0.1 to 2.0 µg/L for the different pharmaceuticals. Relative standard deviations were <26% for all compounds. The procedure was applied to samples from final effluent collected from wastewater treatment plants in Las Palmas de Gran Canaria (Spain), and two compounds were measured at 67 and 113 µg/L in one of them.

  9. Sources of Variability in Chlorophyll Analysis by Fluorometry and by High Performance Liquid Chromatography. Chapter 22

    Science.gov (United States)

    VanHeukelem, Laurie; Thomas, Crystal S.; Glibert, Patricia M.

    2001-01-01

    The need for accurate determination of chlorophyll a (chl a) is of interest for numerous reasons. From the need for ground-truth data for remote sensing to pigment detection for laboratory experimentation, it is essential to know the accuracy of the analyses and the factors potentially contributing to variability and error. Numerous methods and instrument techniques are currently employed in the analyses of chl a. These methods range from spectrophotometric quantification, to fluorometric analysis and determination by high performance liquid chromatography. Even within the application of HPLC techniques, methods vary. Here we provide the results of a comparison among methods and provide some guidance for improving the accuracy of these analyses. These results are based on a round-robin conducted among numerous investigators, including several in the Sensor Intercomparison and Merger for Biological and Interdisciplinary Oceanic Studies (SIMBIOS) and HyCODE Programs. Our purpose here is not to present the full results of the laboratory intercalibration; those results will be presented elsewhere. Rather, here we highlight some of the major factors that may contribute to the variability observed. Specifically, we aim to assess the comparability of chl a analyses performed by fluorometry and HPLC, and we identify several factors in the analyses which may contribute disproportionately to this variability.

  10. Detection of HEMA in self-etching adhesive systems with high performance liquid chromatography

    Science.gov (United States)

    Panduric, V.; Tarle, Z.; Hameršak, Z.; Stipetić, I.; Matosevic, D.; Negovetić-Mandić, V.; Prskalo, K.

    2009-04-01

    One of the factors that can decrease hydrolytic stability of self-etching adhesive systems (SEAS) is 2-hydroxymethylmethacrylate (HEMA). Due to hydrolytic instability of acidic methacrylate monomers in SEAS, HEMA can be present even if the manufacturer did not include it in original composition. The aim of the study was to determine the presence of HEMA because of decomposition by hydrolysis of methacrylates during storage, resulting with loss of adhesion strength to hard dental tissues of the tooth crown. Three most commonly used SEAS were tested: AdheSE ONE, G-Bond and iBond under different storage conditions. High performance liquid chromatography analysis was performed on a Nucleosil C 18-100 5 μm (250 × 4.6 mm) column, Knauer K-501 pumps and Wellchrom DAD K-2700 detector at 215 nm. Data were collected and processed by EuroCrom 2000 HPLC software. Calibration curves were made related eluted peak area to known concentrations of HEMA (purchased from Fluka). The elution time for HEMA is 12.25 min at flow rate 1.0 ml/min. Obtained results indicate that no HEMA was present in AdheSE ONE because methacrylates are substituted with methacrylamides that seem to be more stable under acidic aqueous conditions. In all other adhesive systems HEMA was detected.

  11. Determination of Decabrominated Diphenyl Ether in Soils by Soxhlet Extraction and High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Xing-Jian Yang

    2013-01-01

    Full Text Available This study described the development of a method based on soxhlet extraction combining high performance liquid chromatography (soxhlet-HPLC for the accurate detection of BDE-209 in soils. The solvent effect of working standard solutions in HPLC was discussed. Results showed that 1 : 1 of methanol and acetone was the optimal condition which could totally dissolve the BDE-209 in environmental samples and avoid the decrease of the peak area and the peak deformation difference of BDE-209 in HPLC. The preliminary experiment was conducted on the configured grassland (1 μg/g to validate the method feasibility. The method produced reliable reproducibility, simulated soils (n=4 RSD 1.0%, and was further verified by the analysis e-waste contaminated soils, RSD range 5.9–11.4%. The contamination level of BDE-209 in burning site was consistent with the previous study of Longtang town but lower than Guiyu town, and higher concentration of BDE-209 in paddy field mainly resulted from the long-standing disassembling area nearby. This accurate and fast method was successfully developed to extract and analyze BDE-209 in soil samples, showing its potential use for replacing GC to determinate BDE-209 in soil samples.

  12. Description and validation of coupling high performance liquid chromatography with resonance Rayleigh scattering in aminoglycosides determination

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Lei [Chemistry and Chemical Engineering, Southwest University, 400715 Chongqing (China); Peng Jingdong, E-mail: hxpengjd@swu.edu.cn [Chemistry and Chemical Engineering, Southwest University, 400715 Chongqing (China); Tang Jinxia; Yuan Binfang; He Rongxing; Xiao Ying [Chemistry and Chemical Engineering, Southwest University, 400715 Chongqing (China)

    2011-11-14

    Graphical abstract: Theoretical and experimental analysis had proved that aminoglycosides reacted with Congo red to form binary compounds simultaneously, which led to a novel HPLC-RRS strategy being applied in substances which are not fluorescing and not UV absorbed. Highlights: {yields} A novel HPLC-RRS strategy was shown in this study. {yields} Theoretical and experimental analysis had proved the feasibility of this method. {yields} Because of its specificity, no interference from the matrix was observed. {yields} The analytes in biological matrix were all well resolved without any interference. {yields} It provided new insights for analytes lack of useful spectroscopic and electrochemical properties. - Abstract: In view of the fact that many substances generally exhibit very little ultraviolet absorbance and the absence of native fluorescence, a new strategy with simple instrumentation and excellent analytical performance combining high performance liquid chromatography (HPLC) with resonance Rayleigh scattering (RRS) was developed. It was validated for the quantification of aminoglycosides (AGs). This fact was also carefully calculated by quantum chemistry. However, the sensitivity was probably limited by the volume of flow-through cell. Therefore, the result calls for a suitable one to ensure optimal RRS signal. Interestingly, when serum or urine samples of analytes were analyzed by this method, they were all well resolved without any interference, which would hold a new perspective to be applied in the determination of substances in biological matrix.

  13. Determination of Capsaicin and Dihydrocapsaicin in Capsicum Fruit Samples using High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Ayman Abdel Ghafar

    2011-10-01

    Full Text Available The aim of the present study was to determine the content of capsaicin and dihydrocapsaicin in Capsicum samples collected from city markets in Riyadh (Saudi Arabia, calculate their pungency in Scoville heat units (SHU and evaluate the average daily intake of capsaicin for the population of Riyadh. The investigated samples consisted of hot chillies, red chillies, green chillies, green peppers, red peppers and yellow peppers. Extraction of capsaicinoids was done using ethanol as solvent, while high performance liquid chromatography (HPLC was used for separation, identification and quantitation of the components. The limit of detection (LOD of the method was 0.09 and 0.10 µg/g for capsaicin and dihydrocapsaicin, respectively, while the limit of quantification (LOQ was 0.30 and 0.36 µg/g for capsaicin and dihydrocapsaicin, respectively. Hot chillies showed the highest concentration of capsaicin (4249.0 ± 190.3 µg/g and the highest pungency level (67984.60 SHU, whereas green peppers had the lowest detected concentration (1.0 ± 0.9 µg/g; green peppers, red peppers and yellow peppers were non pungent. The mean consumption of peppers for Riyadh city population was determined to be 15.5 g/person/day while the daily capsaicin intake was 7.584 mg/person/day.

  14. AB063. Prevalence of thalassemias and hemoglobinopathies detected via high performance liquid chromatography in Filipinos

    Science.gov (United States)

    Silao, Catherine Lynn; Fabella, Terence Diane; Yuson, Ernesto; Naranjo, Maria Liza; Padilla, Carmencita

    2015-01-01

    Background The thalassemias and hemoglobinopathies are groups of autosomal recessive inherited blood disorders affecting the quantity and quality of hemoglobin. Patients with the disease can vary from clinically asymptomatic to transfusion dependent individuals. It is considered prevalent in many parts of the world particularly in Southeast Asia. Thus, screening and prevalence determination of these diseases are important in the Filipino population. The study aims to determine the prevalence of thalassemias and hemoglobinopathies in the Philippines using high performance liquid chromatography. Methods Referred patients by hematologists from different parts of the country from October 2008 to December 2014 were included. Peripheral blood extracted from the subjects, were hemolyzed and screened for thalassemias and hemoglobinopathies using VariantTM HPLC. Data interpretations were based on levels of the HbA2 Fetal Hb and HbA detected. Results Majority of the patients were beta thalassemics followed by alpha-thalassemics. Hemoglobin E was found in 1% of the population tested while 2% of the patients have beta thalassemia with HbE interaction. Conclusions A significant proportion of thalassemias and hemoglobinopathies were determined from the 6-year screening of Filipinos using VariantTM HPLC. The results of this study provide not only confirmation of the occurrence and prevalence of these growing and diverse groups of genetic blood diseases but also suggest that the use of HPLC is a useful screening tool.

  15. Quantitative Determination of Compounds from Akebia quinata by High-Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yen, Nguyen; Thu, Nguyen; Zhao, Bing Tian; Woo, Mi Hee; Min, Byung Sun [Catholic Univ. of Daegu, Gyeongsan (Korea, Republic of); Lee, Jae Hyun [Dongguk Univ., Yongin (Korea, Republic of); Kim, Jeong Ah [Kyungpook National Univ., Daegu (Korea, Republic of); Son, Jong Keun [Yeungnam Univ., Gyeongsan (Korea, Republic of); Choi, Jae Sui [Pukyung National Univ., Busan (Korea, Republic of); Woo, Eun Rhan [Chosun Univ., Gwangju (Korea, Republic of)

    2014-07-15

    To provide the scientific corroboration of the traditional uses of Akebia quinata (Thunb.) Decne., a detailed analytical examination of A. quinata stems was carried out using a reversed-phase high performance liquid chromatography (RP-HPLC) method coupled to photodiode array detector (PDA) for the simultaneous determination of four phenolic substances; cuneataside D, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside, 3-caffeoylquinic acid and calceolarioside B. Particular attention was focused on the main compound, 3-caffeoylquinic acid, which has a range of biological functions. In addition, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside was considered as a discernible marker of A. quinata from its easy confuse plants. The contents of compounds 2 and 3 ranged from 0.72 to 2.68 mg/g and from 1.66 to 5.64 mg/g, respectively. The validation data indicated that this HPLC/PDA assay was used successfully to quantify the four phenolic compounds in A. quinata from different locations using relatively simple conditions and procedures. The pattern-recognition analysis data from 53 samples classified them into two groups, allowing discrimination between A. quinata and comparable herbs. The results suggest that the established HPLC/PDA method is suitable for quantitation and pattern-recognition analyses for a quality evaluation of this medicinal herb.

  16. Determination of sulphachloropyrazine-diaveridine residues by high performance liquid chromatography in broiler edible tissues

    Science.gov (United States)

    LI, Yongjun; BU, Shijin

    2015-01-01

    Diaveridine (DVD) is used in combination with sulphachloropyrazine (SPZ) as an effective antibacterial agent and antiprotozoal agent, respectively, in humans and animals. To gain a better understanding of the metabolism of SPZ and DVD in the food-producing animals, a high performance liquid chromatography (HPLC) method to determine and quantify sulphachloropyrazine (SPZ) and diaveridine (DVD) suspension residues from broilers is reported. Thirty healthy chickens were orally administered with sulphachloropyrazine-diaveridine (SPZ-DVD) suspension in water of 300 mg/l (SPZ) per day for seven successive days. Six chickens per day were slaughtered at 0, 1, 3, 5 and 7 days after the last administration. This procedure permitted SPZ and DVD to be separated from muscle tissue, liver, kidneys and skin with fat after extraction with acetonitrile and acetone under slightly acidic conditions. From the detected residuals in different tissues, we found that SPZ was quickly eliminated in liver and muscle, and slowly eliminated in kidney and skin with fat. DVD was quickly eliminated in liver and slowly eliminated in kidney. The withdrawal period of SPZ was 3.26, 3.72, 4.39 and 5.43 days in muscle, liver, kidney and skin with fat, respectively. The withdrawal period of DVD was 4.77, 4.94, 6.74 and 4.58 days in muscle, liver, kidney and skin with fat, respectively. Therefore, the suggested withdrawal period for SPZ-DVD suspension should be 7 days after dosing for seven successive days. PMID:26212255

  17. Analysis of Fluconazole in Human Urine Sample by High Performance Liquid Chromatography Method

    Science.gov (United States)

    Hermawan, D.; Ali, N. A. Md; Ibrahim, W. A. Wan; Sanagi, M. M.

    2013-04-01

    A method for determination of fluconazole, antifungal drug in human urine by using reversed-phased high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detector was developed. Optimization HPLC conditions were carried out by changing the flow rate and composition of mobile phase. The optimum separation conditions at a flow rate 0.85 mL/min with a composition of mobile phase containing methanol:water (70:30, v/v) with UV detection at a wavelength 254 nm was able to analyze fluconazole within 3 min. The excellent linearity was obtained in the range of concentration 1 to 10 μg/mL with r2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 μg/mL and 1.28 μg/mL, respectively. Solid phase extraction (SPE) method using octadecylsilane (C18) as a sorbent was used to clean-up and pre-concentrated of the urine sample prior to HPLC analysis. The average recoveries of fluconazole in spiked urine sample was 72.4% with RSD of 3.21% (n=3).

  18. Determination of multiple human arsenic metabolites employing high performance liquid chromatography inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Stice, Szabina; Liu, Guangliang; Matulis, Shannon; Boise, Lawrence H.; Cai, Yong

    2016-01-01

    During the metabolism of different arsenic-containing compounds in human, a variety of metabolites are produced with significantly varying toxicities. Currently available analytical methods can only detect a limited number of human metabolites in biological samples during one run due to their diverse characteristics. In addition, co-elution of species is often unnoticeable with most detection techniques leading to inaccurate metabolic profiles and assessment of toxicity. A high performance liquid chromatography inductively coupled mass spectrometry (HPLC-ICP-MS) method was developed that can identify thirteen common arsenic metabolites possibly present in human with special attention dedicated to thiolated or thiol conjugated arsenicals. The thirteen species included in this study are arsenite (AsIII), arsino-glutathione (As(GS)3), arsenate (AsV), monomethylarsonous acid (MMAIII), monomethylarsino-glutathione (MMAIII(GS)2), monomethylarsonic acid (MMAV), dimethylarsinous acid (DMAIII (from DMAIIII)), S-(dimethylarsinic)cysteine (DMAIII(Cys)), dimethylarsino-glutathione (DMAIII(GS)), dimethylarsinic acid (DMAV), dimethylmonothioarsinic acid (DMMTAV), dimethyldithioarsinic acid (DMDTAV), dimethylarsinothioyl glutathione (DMMTAV(GS)). The developed method was applied for the analysis of cancer cells that were incubated with Darinaparsin (DMAIII(GS)), a novel chemotherapeutic agent for refractory malignancies, and the arsenic metabolic profile obtained was compared to results using a previously developed method. This method provides a useful analytical tool which is much needed in unequivocally identifying the arsenicals formed during the metabolism of environmental arsenic exposure or therapeutic arsenic administration. PMID:26708625

  19. A novel high-performance liquid chromatography fingerprint approach to discriminate Phyllostachys pubescens from China

    Directory of Open Access Journals (Sweden)

    Jin Yong-Chun

    2012-01-01

    Full Text Available Background: A high-performance liquid chromatography fingerprint of different variants of Phyllostachys pubescens was developed for the source discrimination and quality control of Phyllostachys pubescens medicines produced in Zhejiang Province, China. Materials and Methods: Samples of Phyllostachys pubescens collected from nine cultivars in Zhejiang Province were used to establish the fingerprint. Taking the chromatographic peak (isoorientin as the reference peak, the chromatographic column was Sunfire C 18 ODS (250 mm×4.6 mm, 5 ΅m at a column temperature of 25°C. The mobile phase was acetonitrile 0.8% acetic acid water solution (in a gradient elution mode at a flow rate of 1 ml/min. The detection wavelength was 330 nm. Results: 20 common peaks were established in the chromatographic fingerprints of Phyllostachys pubescens. And then by comparing the UV and standard substance with those of the authentic standards and literature, eight main peaks in the fingerprints were identified. Data of nine cultivars were evaluated statistically using similarity analysis, hierarchical cluster analysis (HCA in order to establish a similarity standard of fingerprint for quality control of Phyllostachys pubescens, then to classify the samples. The similarity indexes were all above 0.95 between reference chromatogram and each sample′s chromatogram. Conclusion: in this study, the methods established are reliable, and could be used to evaluate the quality and to identify the species of Phyllostachys pubescens in the future.

  20. Determination of capsaicin and dihydrocapsaicin in Capsicum fruit samples using high performance liquid chromatography.

    Science.gov (United States)

    Al Othman, Zeid Abdullah; Ahmed, Yacine Badjah Hadj; Habila, Mohamed Abdelaty; Ghafar, Ayman Abdel

    2011-10-24

    The aim of the present study was to determine the content of capsaicin and dihydrocapsaicin in Capsicum samples collected from city markets in Riyadh (Saudi Arabia), calculate their pungency in Scoville heat units (SHU) and evaluate the average daily intake of capsaicin for the population of Riyadh. The investigated samples consisted of hot chillies, red chillies, green chillies, green peppers, red peppers and yellow peppers. Extraction of capsaicinoids was done using ethanol as solvent, while high performance liquid chromatography (HPLC) was used for separation, identification and quantitation of the components. The limit of detection (LOD) of the method was 0.09 and 0.10 µg/g for capsaicin and dihydrocapsaicin, respectively, while the limit of quantification (LOQ) was 0.30 and 0.36 µg/g for capsaicin and dihydrocapsaicin, respectively. Hot chillies showed the highest concentration of capsaicin (4249.0 ± 190.3 µg/g) and the highest pungency level (67984.60 SHU), whereas green peppers had the lowest detected concentration (1.0 ± 0.9 µg/g); green peppers, red peppers and yellow peppers were non pungent. The mean consumption of peppers for Riyadh city population was determined to be 15.5 g/person/day while the daily capsaicin intake was 7.584 mg/person/day.

  1. [Determination of six pesticides in milk using cloud point extraction-high performance liquid chromatography].

    Science.gov (United States)

    Wang, Jian; Cui, Yanmei; Liu, Wei; Yang, Mingmin; Chen, Jianbo

    2007-11-01

    The feasibility of employing cloud point extraction (CPE) as extraction and preconcentration method for the recovery of herbicides from milk samples followed by high performance liquid chromatography (HPLC) analysis is demonstrated. An aqueous surfactant solution containing 60 g/L Tween 20 or Triton X-100 was heated with an appropriate concentration of (NH4)2SO4 or NaCl for the extraction of herbicides. The extract was analyzed by HPLC subsequently. Six herbicides in milk were analyzed simultaneously. The results showed that the linear dynamic ranges of detection were 20 - 10 000 microg/L for tralkoxydim, metribuzin and bromoxynil, 30 - 10 000 microg/L for mefenacet, and 50 - 10 000 microg/L for bensulfuron-methyl and nicosulfuron. The correlation coefficients were 0.998 1 - 0.999 7. The average recoveries of the six herbicides ranged from 85.09% to 96.74%. The relative standard deviations for the six herbicides were in the range of 1.90% - 3.98%. The limits of detection for the six pesticides were lower than the maximum residue limits (MRL) of China. The results indicate that the method is easier, faster, sensitive and produces less pollutants.

  2. Analysis of ciprofloxacin by a simple high-performance liquid chromatography method.

    Science.gov (United States)

    Wu, Shihn-Sheng; Chein, Chih-Yuan; Wen, Yen-Hsia

    2008-07-01

    A simple and sensitive high-performance liquid chromatographic method is described for the quantitative analysis of ciprofloxacin in pharmaceuticals and human plasma. The method employs reversed-phase chromatography using an RP-C18 column with an isocratic mobile phase of acetonitrile-2% acetic acid aqueous solution (16:84, v/v), umbelliferone as an internal standard, and a flow rate of 1.0 mL/min. The UV detector is set at 280 nm. The limit of detection is 0.25 microM (S/N = 3, injection volume = 10 microL). The regression equations are linear (r > 0.9999) over a range between 0.51 approximately 130 microM for the pharmaceutical analysis of ciprofloxacin and 0.51 approximately 64.8 microM for the biological analysis of ciprofloxacin in human plasma. The intra- and inter-day relative standard deviation and relative error are less than 3.39% and 5.71%, respectively. All the recoveries are greater than 93.8%. This method is successfully applied in a pharmacokinetic study of a volunteer who receives a 500 mg ciprofloxacin tablet.

  3. Simultaneous Determination of Potassium Sorbate and Sodium Benzoate in Doogh Using High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    S. Sohrabvandi

    2015-09-01

    Full Text Available In this research, high performance liquid chromatography (HPLC as a simple and rapid technique was used for the determination of potassium sorbate and sodium benzoate in different brands of Doogh (typical Iranian drink based on fermented milk. The chromatographic separation was achieved with a C18 column (250 mm×4 I.D, 5 µm and one buffered mobile phase, acetate buffer (0.2 mol/L, pH4.4: acetonitrile (63:37 at a flow rate of 1 mL/min. The effluent was monitored at 235nm, respectively. The main affecting factors, such as Carrez solution amount, pH and centrifuge speed were optimized. Limits of detection (LODs were 1.823 for sorbic acid and 1.985 for benzoic acid. Relative standard deviations (RSDs for quintuplicate analyses were 4.4 for sorbic acid and 4.087 for benzoic acid. The method also showed good linearity in a range from 4 to 1000 mg/L with correlation coefficients (R2 of 0.990 for sorbic acid and 0.995 for benzoic acid. Recoveries for the two analytes were 80 for sorbic acid and 65 for benzoic acid. Comparing to the other techniques, the proposed method was significantly less time-consuming and had more acceptable accuracy, precision and interruption elimination in samples. The developed method was successfully used for the routine monitoring of benzoate and sorbate in Doogh.

  4. High-performance liquid chromatography of unmodified rosin and its applications in contact dermatology.

    Science.gov (United States)

    Sadhra, S; Gray, C N; Foulds, I S

    1997-10-24

    Rosin is a well recognised skin sensitiser and is also amongst the most common causes of occupational asthma. Due to its complex chemical composition, it is difficult to isolate its many components and this has hindered progress in the identification of the specific respiratory and contact allergens it contains. This paper reports the application of high-performance liquid chromatography and other analytical techniques to the isolation and identification of contact allergens in complex mixtures such as rosin. HPLC methods were developed in order to isolate as many rosin components as possible and these were then patch tested on rosin sensitive individuals. The structure of the most dermatologically active component was then determined using mass spectrometry, nuclear magnetic resonance and infrared techniques. An HPLC method has also been developed which will enable the identification of rosin in commercial products, providing a valuable tool for determining the cause of rosin contact allergy. Furthermore, mass spectral data for the common abieitic-type resin acids are compiled which were used to confirm the identification of the HPLC resin acid peaks and have not been reported previously.

  5. Quantitation of aflatoxins in walnut kernels by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Kabak, Bulent

    2014-01-01

    A total of 85 walnut samples collected between October 2012 and April 2013 in different provinces of Turkey were analysed for the presence of aflatoxins (AFs). The method involved methanol-water extraction, clean-up with immunoaffinity columns and a sensitive high-performance liquid chromatography coupled with fluorescence detection after post-column derivatisation. The method was validated for selectivity, linearity, trueness, precision, limit of detection and limit of quantification (LOQ), which met the performance criteria as set by EC regulation No. 401/2006. LOQs were 0.07, 0.04, 0.09 and 0.05 µg kg(-1) for AFB1, AFB2, AFG1 and AFG2, respectively. AFs were present in 9.4% of walnut samples (8/85) at total AFs levels ranging from 0.09 to 15.4 µg kg(-1). Only one of eight walnut samples exceeded the European Union limit of 2 and 4 µg kg(-1) for AFB1 and total AFs, respectively.

  6. Determination of Benzalkonium Chloride in Nasal Drops by High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Danijela A. Kostić

    2012-01-01

    Full Text Available A high-performance liquid chromatography (HPLC system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC in nosal drops. A Chromolit RP-18e, 100 x 4.6, (UM6077/035 column was used at 40 °C. The mobile phase, optimized through an experimental design, was a 70:30 (v/v mixture of 0.057M Na-heksansulphonate potassium, dihydrogen orthophosphate buffer (pH 2.9 and acetonitrile, pumped at a flow rate of 1.75 mL/min at maintaining column temperature at 40 °C. Maximum UV detection was achieved at 215 nm. The method was validated in terms of selectivity, linearity, repeatability, precision and accuracy. The method was successfully applied for the determination of BKC in a pharmaceutical formulation of nasal drop solution without any interference from common excipients and drug substance. All the validation parameters were within the acceptance range, concordant to ICH guidelines.

  7. Determination of benzalkonium chloride in viscous ophthalmic drops of azithromycin by high-performance liquid chromatography *

    Science.gov (United States)

    Shen, Yan; Xu, Sheng-jie; Wang, Shi-chun; Tu, Jia-sheng

    2009-01-01

    A high-performance liquid chromatography (HPLC) system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC) in azithromycin viscous ophthalmic drops. A Venusil-XBP(L)-C18 (150 mm×4.6 mm, 5 μm) column was used at 50 °C. The mobile phase consisted of a mixture of methanol-potassium phosphate (16:5, v/v). Two sample preparation methods were compared. The results suggested that, compared with an extraction procedure, a deproteinization procedure was much quicker and more convenient. Using the deproteinization procedure for sample preparation, calibration curves were linear in the range 5.0~50 μg/ml. The within-day and inter-day coefficients of variation were less than 10%. The average recoveries were determined as 96.70%, 98.52%, and 97.96% at concentrations of 10.0, 30.0, and 50.0 μg/ml, respectively. Variability in precision did not exceed 5%. In conclusion, this HPLC method using a simple sample treatment procedure appears suitable for monitoring BKC content in azithromycin viscous ophthalmic drops. PMID:19946951

  8. Quantification of mRNA by RT-competitive-PCR and high performance liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The use of RT-competitive-PCR with high performance liquid chromatography (HPLC) detection to quantify the absolute number of mRNA copies in mammalian cells is reported. As an example, the glutathione transferase (GST)-α mRNA in human hepatoma Hep G2 cells has been estimated. A PCR-generated internal standard was used as a competitor, co-amplified with the GST-α target sequence. The RT-competitive-PCR method was improved by designing target and competitor molecules which differed in only 30 base pairs. This allowed the two sequences to be co-amplified with the same efficiency. This improvement also facilitated a wider ratio to be used than previous methods (target:competitor ratio between 0.2 and 5). Products were baseline separated by HPLC using an ion-exchange column readily quantified at 260 nm. To validate the improved methodology, the effect of a known GST-α inducer, the anticancer drug oltipraz, was shown to induce GST-α mRNA up to 3-fold in Hep G2 cells. The RT-competitive PCR-HPLC method provides a reliable and sensitive way to quantify the amount of specific mRNA with 0.1 ng of total RNA.

  9. Chemical fingerprint analysis of Gentianae Radix et Rhizoma by high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Baozhong Duan

    2012-02-01

    Full Text Available Gentianae Radix et Rhizoma (also called “Longdan” in Chinese is commonly used for eliminating damp-heat and quenching the fire of liver and gall bladder in traditional Chinese medicine. In this study, a novel and reliable method using high-performance liquid chromatography (HPLC was developed both for quantitative analysis of four bioactive compounds (loganic acid, swertiamarin, gentiopicroside and sweroside and chemical fingerprint analysis of “Longdan”. In quantitative analysis, four compounds showed good regressions (R2>0.9987 within the test ranges and the recovery of the method was in the range 97.61−102.49%. In fingerprint analysis, ten characteristic peaks were selected to evaluate the similarities of the crude drugs, and the HPLC chromatograms of twenty samples from different regions of China showed similar patterns. The results demonstrated that the combination of the quantitative and chromatographic fingerprint analyses offered an efficient way to evaluate the quality consistency of Gentianae Radix et Rhizoma.

  10. High performance liquid chromatography determination of theobromine and caffeine in cocoa beans gamma irradiated

    Energy Technology Data Exchange (ETDEWEB)

    Soares, Anderson D.B. [Faculdade de Engenharia de Varginha, MG (Brazil); Mansur Neto, Elias [Minas Gerais Univ., Belo Horizonte, MG (Brazil)

    1997-12-01

    Irradiation is a processing technology that has been shown to be a wholesome process by many scientific studies conducted worldwide during the past 40 years, which has been approved by 37 countries. Irradiated foods have been studied so extensively, that the effects on foods are better understood than any other preservation process, including food freezing and dehydration. Cocoa beans has been commercially irradiated in countries such as Ivory Coast and Argentina. The alkaloids theobromine and caffeine are responsible for the mildly stimulating properties and bitter taste of cocoa and chocolate products. Previously fermented dried and nonfumigated cocoa beans were irradiated at doses of 0, 5.0, 10.0 and 20.0 kGy using Co-60 gamma rays. The samples were analysed for determining theobromine and caffeine contents in the cocoa beans by TIMBIE et al. (1978) high performance liquid chromatography (HPLC) method. Boiling water extracts were cooled, centrifuged and injected into the chromatograph. Theobromine and caffeine were quantitated at 273 nm and showed the tendency of decreasing as the dose of radiation increases. Theobromine and caffeine ranged from 42.3 to 37.1 mg/g and from 7.60 to 6.13 mg/g. respectively from 0 to 20.0 kGy. These results were discussed in relation to the possible acceptance of radiosterization of cocoa beans commercially up to the dose of 20.0 kGy. (author). 10 refs., 1 tab.

  11. Preparation and Characterization of a New Quercetin-bonded Stationary Phase for High Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    李来生; 方奕珊; 陈红; 张杨

    2012-01-01

    A quercetin-bonded silica gel stationary phase (QUSP) containing natural flavonoid ligand was first prepared via γ-glycidoxypropyltrimethoxysilane (KH-560) as a coupling reagent for high-performance liquid chromatography. Its chemical structure was characterized by Fourier infrared spectroscopy, elemental analysis, thermal thermogravimetry and 13C cross polarization/magic angle spinning nuclear magnetic resonance (CP/MAS NMR). The chromatographic property of QUSP was systematically evaluated by using neutral, basic and acidic aromatic com- pounds as probes. In order to clarify its retention mechanism, a comparative study of QUSP with conventional oc- tadecylsilyl-bonded stationary phase (ODS) was also carried out under the same conditions. The results showed that the new quercetin-bonded phase exhibited an excellent reversed-phase chromatographic property with relatively weak hydrophobicity. However, it has an advantage over ODS in the fast separation of polar aromatic compounds because the quercetin ligand could provide various sites besides hydrophobicity, such as hydrogen bonding, dipole-dipole, n-n staking and charge transfer interactions. QUSP was performed in the baseline separations of ion- ized polar basic or acidic compounds, including pyridines, anilines, pyrimidines, purines and phenols with symmet- ric peak shape in common mobile phases without buffer salt within relatively short time. The natural ligands from herbs are readily available and contain a variety of active sites, which facilitate the exploration of industrial chromatographic separation materials for green products.

  12. Determination of folates in seaweeds by high-performance liquid chromatography.

    Science.gov (United States)

    Rodríguez-Bernaldo de Quirós, A; Castro de Ron, C; López-Hernández, J; Lage-Yusty, M A

    2004-04-02

    A reversed-phase high-performance liquid chromatography (HPLC) method, with a combination of fluorescence and ultraviolet detectors, to determine the folate forms present in commercial macroalgae products form northwest Spain as part of nutritional studies in dehydrated and canned seaweeds is reported. The method includes extraction of folates from seaweed by heat treatment, deconjugation of folate polyglutamates by incubation with hog kidney conjugase and purification by solid-phase extraction (SPE) with strong anion-exchange (SAX) cartridges. Separation was achieved with a Tracer Extrasil ODS 5 microm 25 cm x 0.4 cm column using acetonitrile and potassium phosphate buffer (pH 2.21 as mobile phase. Good results were obtained with respect to repeatability (relative standard deviation (R.S.D.) or = 90.80%). The amount of folate (as folic acid) in the six species ranged from 61.4 to 161.6 microg per 100 g dry mass. In all the seaweeds studied (Himanthalia elongata, Laminaria ochroleuca, Palmaria spp., Undaria pinnatifida and Porphyra spp. and Saccorhiza polychides) the single most abundant form is 5-CH3-H4-folate, except Porphyra and Himanthalia.

  13. Simultaneous determination of thiamine and riboflavin in edible marine seaweeds by high-performance liquid chromatography.

    Science.gov (United States)

    Sánchez-Machado, D I; López-Cervantes, J; López-Hernández, J; Paseiro-Losada, P

    2004-03-01

    This study presents a high-performance liquid chromatography (HPLC) method for simultaneous determination of thiamine and riboflavin and the results of its application to a number of edible seaweeds that are sampled in dried form (Himanthalia elongata, Laminaria ochroleuca, Undaria pinnatifida, Palmaria sp., and Porphyra sp.) or as canned food (H. elongata and Saccorhiza polyschides). Samples are prepared by acid and enzymatic hydrolysis. Optimized conditions for reversed-phase HPLC with fluorescence detection are as follow: column, Kromasil 100 C18; column temperature, 35 degrees C; mobile phase, a 72:28 (v/v) mixture of 0.005 M ammonium acetate (pH 6.7)-methanol; and flow rate, 1.35 mL/min. With these conditions, recovery is 95.52% for thiamine and 90.08% for riboflavin, and the method precision (relative standard deviation) is 2.66% for thiamine and 2.21% for riboflavin. On a dry weight basis, thiamine contents range from 0.14 microg/g in dried H. elongata to 2.02 microg/g in dried Porphyra and riboflavin contents from 0.31 microg/g in canned H. elongata to 6.15 microg/g in dried Porphyra.

  14. Simultaneous determination of eleven characteristic lignans in Schisandra chinensis by high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Junyang Hu

    2013-01-01

    Full Text Available Background: Schisandra chinensis, one of the well-known traditional Chinese herbal medicines, is derived from the dry ripe fruits of Schisandra chinensis (Turcz. Baill. according to the 9th China Pharmacopeia. Lignans are the main components isolated from extracts of S. chinensis and their content varies depending on where S. chinensis was collected. We have established a qualitative and quantitative method based on the bioactive lignans for control of the quality of S. chinensis from different sources. Materials and Methods: To develop a high-performance liquid chromatography method, an Elite ODS C18 column (250 mm Χ 4.6 mm, 5μm at a column temperature of 30°C and flow rate of 1.0ml/min using acetonitrile (A and water (B as the mobile phase with a linear gradient and the peaks were monitored at 217 nm. Results: All calibration curves showed good linearity (r ≥ 0.9995 within test ranges. This method showed good repeatability for the quantification of these eleven components in S. chinensis with intra- and inter-day relative standard deviations less than 0.43% and 1.21%, respectively. In the recovery test, results of accuracy ranged from 99.51% to 101.31% with RSD values less than 2.68%, Conclusion: The validated method can be successfully applied to quantify the eleven investigated components in 22 samples of S. chinensis from different sources.

  15. A stability-indicating high performance liquid chromatography method to determine apocynin in nanoparticles

    Directory of Open Access Journals (Sweden)

    Juliana Kovalczuk de Oliveira

    2017-04-01

    Full Text Available In this study, we developed and validated a fast, specific, sensitive, precise and stability-indicating high performance liquid chromatography (HPLC method to determine the drug apocynin in bovine serum albumin (BSA nanoparticles. Chromatographic analyses were performed on an RP C18 column and using a photodiode array detector at a wavelength of 276 nm. Mobile phase consisted of a mixture of acetonitrile and 1% acetic acid (60:40, v/v, and it was eluted isocratically at a flow rate of 0.8 mL/min. The retention time of apocynin chromatographic peak was 1.65 min. The method was linear, precise, accurate and specific in the range of 5–100 μg/mL. The intra- and inter-day precisions presented relative standard deviation (RSD values lower than 2%. The method was robust regarding changes in mobile phase proportion, but not for flow rate. Limits of detection and quantitation were 78 ng/mL and 238 ng/mL, respectively. Apocynin was exposed to acid and alkali hydrolysis, oxidation and visible light. The drug suffered mild degradation under acid and oxidation conditions and great degradation under alkali conditions. Light exposure did not degrade the drug. The method was successfully applied to determine the encapsulation efficiency of apocynin in BSA nanoparticles.

  16. Determination of Residual Acrylamide in Medical Polyacrylamide Hydrogel by High Performance Liquid Chromatography tandem Mass Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    WEI-WEI LI; HUI LI; ZHI-FEI LIU; QUN QIAO

    2009-01-01

    Objective To determine residual acrylamide in medical polyacrylamide hydrogel by high performance liquid chromatography tandem mass spectroscopy (HPLC-MS). Methods After 13C3 labeled acrylamide was added, the sample was extracted with water and then cleaned up with ExtrelutTM 20. The polyaerylamide hydrogel sample and 20 clinical cases were analyzed by HPLC-MS/MS and isotope dilution quantifying technique in selected reaction monitoring (SRM) mode. Results Acrylamide was separated from polyacrylamide hydrogel. The concentration of acrylamide in polyacrylamide hydrogel ranged from 3.9×109 to 3.1×108g/L in the 20 clinical cases. The peak area was favorable linear and the range was up to 3 000 μg/L. The recovery rate was 103.1% with a relative standard deviation (RSD) of 6.20%, when the mark level was 50 μg/L. Conclusion HPLC-MS is a rapid, accurate, and sensitive method for the determination of residual acrylamide in medical polyacrylamide hydrogel.

  17. A universal, high recovery assay for protein quantitation through temperature programmed liquid chromatography (TPLC).

    Science.gov (United States)

    Orton, Dennis J; Doucette, Alan A

    2013-03-15

    As an alternative to direct UV absorbance measurements, estimation of total protein concentration is typically conducted through colorimetric reagent assays. However, for protein-limited applications, the proportion of the sample sacrificed to the assay becomes increasingly significant. This work demonstrates a method for quantitation of protein samples with high recovery. Temperature programmed liquid chromatography (TPLC) with absorbance detection at 214nm permits accurate estimation of total protein concentration from samples containing as little as 0.75μg. The method incorporates a temperature gradient from 25 to 80°C to facilitate elution of total protein into a single fraction. Analyte recovery, as measured from 1 and 10μg protein extracts of Escherichia coli, is shown to exceed 93%. Extinction coefficients at 214nm were calculated across the human proteome, providing a relative standard deviation of 21% (versus 42% at 280nm), suggesting absorbance values at 214nm provide a more consistent measure of protein concentration. These results translate to a universal protein detection strategy exhibiting a coefficient of variation below 10%. Together with the sensitivity and tolerance to contaminants, TPLC with UV detection is a favorable alternative to colorimetric assay for total protein quantitation, particularly in sample-limited applications.

  18. Determination of acrylamide monomer in polyacrylamide degradation studies by high-performance liquid chromatography.

    Science.gov (United States)

    Ver Vers, L M

    1999-12-01

    A high-performance liquid chromatography method using C18 and ion-exchange columns in series is developed for the determination of acrylamide and acrylic acid monomers in polymeric samples. The C18 column acts as a guard column, trapping surfactants and impurities and retaining the nonionic species. The ion-exchange column then separates the monomers according to their respective ionic strengths. This method has been proven in the laboratory to work successfully for all types of acrylamide/acrylic acid polymers and matrices. Detection limits for both monomers can be achieved in the parts-per-billion range. The method is used to study the possible degradation of polyacrylamide to acrylamide monomer in the presence of glyphosate (a herbicide) and sunlight. Polyacrylamide is used as a spray drift reduction aid in combination with glyphosate. In normal applications, the polymer and herbicide are in contact with each other in the presence of sunlight. The results show that the polymer does not degrade to acrylamide in the presence of glyphosate or sunlight or any combination of the two. It is also observed that glyphosate influences the solubility of polyacrylamide, and care must be used when combining the two.

  19. Determination of Flurbiprofen in Human Plasma by High-Performance Liquid Chromatography.

    Science.gov (United States)

    Yilmaz, Bilal; Erdem, Ali Fuat

    2015-10-01

    A simple high-performance liquid chromatography method has been developed for determination of flurbiprofen in human plasma. The method was validated on an Ace C18 column using UV detection. The mobile phase was acetonitrile-0.05 M potassium dihydrogen phosphate solution (60:40, v/v) adjusted to pH 3.5 with phosphoric acid. The calibration curve was linear between the concentration range of 0.10-5.0 μg/mL. Intra- and inter-day precision values for flurbiprofen in plasma were <4.47, and accuracy (relative error) was better than 3.67%. The extraction recoveries of flurbiprofen from human plasma were between 93.0 and 98.9%. The limits of detection and quantification of flurbiprofen were 0.03 and 0.10 μg/mL, respectively. In addition, this assay was applied to determine the pharmacokinetic parameters of flurbiprofen in six healthy Turkish volunteers who had been given 100 mg flurbiprofen.

  20. Determination of organic mercury species in soils by high-performance liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Hempel, M; Hintelmann, H; Wilken, R D

    1992-03-01

    Reversed-phase high-performance liquid chromatography with ultraviolet detection was optimized for the simultaneous separation and quantification of nine organic mercury compounds: methyl-, ethyl-, phenyl-, methoxyethyl-, ethoxyethyl-, benzoic and tolylmercury, mersalylic acid and nitromersol. The nine compounds were successfully separated on octadecylsilane columns (200 x 3 mm i.d.) by gradient elution with a methanol-water mixture ranging from 30 to 50% v/v. The detection limits for the various compounds are in the range 7.0-95.1 micrograms dm-3. For the extraction of five organomercurials from spiked soils, eight different extraction solutions were tested to differentiate between the total content and the available/soluble fraction of the analytes. Ammonium acetate solutions (1 mol dm-3) and water proved to be suitable agents for the estimation of the available and soluble fractions of methyl-, ethyl-, benzoic, methoxyethyl- and ethoxyethylmercury. For the determination of the total content of methyl- and benzoic mercury in soils, solutions of potassium iodide (1 mol dm-3)-ascorbic acid (0.1 mol dm-3) and oxalic acid (1 mol dm-3) provided recoveries in the ranges 53-81%. None of the solutions tested is suitable for the extraction of ethyl-, methoxyethyl- and ethoxyethylmercury.

  1. [Determination of clavulanic acid residue in milk by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Yang, Gang; Huang, Xianhui; Guo, Chunna; Fang, Qiuhua; He, Limin

    2012-06-01

    An analytical method was developed for the determination of clavulanic acid (CLAV) in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A 2 g milk sample was deproteinized by ethanol. The supernatant was transferred into a pear-shaped bottle to be evaporated to about 0.5 mL, and the residue was dissolved with ammonium acetate solution. The sample was determined by HPLC-MS/MS after the purification. The chromatographic separation was achieved on a Luna 5u C8 column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. The identification of CLAV was carried out by MS/MS equipped with electrospray ionization in negative scanning and multiple reaction monitoring (MRM) modes. Matrix-matched calibration standard was used for the quantification. The calibration curve showed perfect linear in the range of 10 - 400 microg/kg with the correlation coefficient of 0.999. The limit of detection (LOD, S/N > or = 3) was 10 microg/kg in milk, and the limit of quantification (LOQ, S/N > or = 10) was 20 microg/kg. The mean recoveries varied from 80.00% to 91.25% at the four spiked levels of LOQ, 1/2MRL (the maximum residue limit), MRL, and 2MRL with the relative standard deviations of 5.60% -8.77%. In conclusion, the established method can be applied for the determination of CLAV residues in milk.

  2. Advances in liquid chromatography-high-resolution mass spectrometry for quantitative and qualitative environmental analysis.

    Science.gov (United States)

    Aceña, Jaume; Stampachiacchiere, Serena; Pérez, Sandra; Barceló, Damià

    2015-08-01

    This review summarizes the advances in environmental analysis by liquid chromatography-high-resolution mass spectrometry (LC-HRMS) during the last decade and discusses different aspects of their application. LC-HRMS has become a powerful tool for simultaneous quantitative and qualitative analysis of organic pollutants, enabling their quantitation and the search for metabolites and transformation products or the detection of unknown compounds. LC-HRMS provides more information than low-resolution (LR) MS for each sample because it can accurately determine the mass of the molecular ion and its fragment ions if it can be used for MS-MS. Another advantage is that the data can be processed using either target analysis, suspect screening, retrospective analysis, or non-target screening. With the growing popularity and acceptance of HRMS analysis, current guidelines for compound confirmation need to be revised for quantitative and qualitative purposes. Furthermore, new commercial software and user-built libraries are required to mine data in an efficient and comprehensive way. The scope of this critical review is not to provide a comprehensive overview of the many studies performed with LC-HRMS in the field of environmental analysis, but to reveal its advantages and limitations using different workflows.

  3. Biogenic amines in table olives. Analysis by high-performance liquid chromatography.

    Science.gov (United States)

    Hornero-Méndez, D; Garrido-Fernández, A

    1994-09-01

    Biogenic amines in fermented vegetables have scarcely been studied. Available data show that in table olives and fermented cucumbers their presence is rare and any determinations made have been restricted mainly to histamine. However, some microorganisms, especially those related to spoilage, found in the fermentation brines of such products may have amino acid decarboxylase activity and give rise to biogenic amines by unusual processes. A method for the simultaneous determination of eight biogenic amines (tryptamine, beta-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine, and spermine) has been developed to study their occurrence in fermented vegetables in more detail. The method consists of extraction of the amines from olive paste with 5% m/v trichloracetic acid and successive transfers into water-saturated n-BuOH and 0.1 mol l-1 HCl. An aliquot of this mixture is dried and derivatized with dansyl chloride. The dansyl derivatives are then analysed by high-performance liquid chromatography. Special emphasis has been given to optimization of the n-BuOH and 0.1 mol l-1 HCl extractions and to the derivatization conditions. By applying this method to the analysis of spoilt olives, the presence of some biogenic amines has been demonstrated. Thus a new method for monitoring the presence of biogenic amines during the fermentation of olives and for detecting anomalous fermentations is envisaged.

  4. Molecular monitoring of the intestinal flora by denaturing high performance liquid chromatography.

    Science.gov (United States)

    Goldenberg, Oliver; Herrmann, Stefanie; Marjoram, Gina; Noyer-Weidner, Mario; Hong, George; Bereswill, Stefan; Göbel, Ulf B

    2007-01-01

    Gut flora analysis is hampered by the complexity of the intestinal microbiota and by inherent limitations of culture-based approaches. Therefore, culture-independent molecular methods based upon 16S rRNA gene analysis were applied successfully for the analysis of complex microbial communities. However, generally accepted and validated profiling methods such as denaturing and temperature gradient gel electrophoresis (DGGE/TGGE) are still laborious and time consuming. Thus, we adapted the separation of amplified bacterial 16S rRNA gene fragments by denaturing high performance liquid chromatography (DHPLC) using the WAVE Microbial Analysis System as a rapid and convenient means to display complex intestinal bacterial communities and to monitor changes in the gut flora. The separation of 16S rRNA gene fragments amplified from reference strains representing main gut bacterial populations and from human stool samples revealed that DHPLC analysis effectively detects bacterial groups predominant in the human gut flora. The investigation of faecal samples from hospitalized patients before, during and after antibiotic therapy showed that PCR-based DHPLC can be used to monitor gut flora changes. Results from DHPLC analysis were comparable with DGGE profiles generated from the same samples, demonstrating that the adapted DHPLC protocol is well suited for the analysis of complex microbial communities.

  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: 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. Determination of xanthohumol in beer based on cloud point extraction coupled with high performance liquid chromatography.

    Science.gov (United States)

    Chen, Ligang; Zhao, Qi; Jin, Haiyan; Zhang, Xiaopan; Xu, Yang; Yu, Aimin; Zhang, Hanqi; Ding, Lan

    2010-04-15

    A method based on coupling of cloud point extraction (CPE) with high performance liquid chromatography separation and ultraviolet detection was developed for determination of xanthohumol in beer. The nonionic surfactant Triton X-114 was chosen as the extraction medium. The parameters affecting the CPE were evaluated and optimized. The highest extraction yield of xanthohumol was obtained with 2.5% of Triton X-114 (v/v) at pH 5.0, 15% of sodium chloride (w/v), 70 degrees C of equilibrium temperature and 10 min of equilibrium time. Under these conditions, the limit of detection of xanthohumol is 0.003 mg L(-1). The intra- and inter-day precisions expressed as relative standard deviations are 4.6% and 6.3%, respectively. The proposed method was successfully applied for determination of xanthohumol in various beer samples. The contents of xanthohumol in these samples are in the range of 0.052-0.628 mg L(-1), and the recoveries ranging from 90.7% to 101.9% were obtained. The developed method was demonstrated to be efficient, green, rapid and inexpensive for extraction and determination of xanthohumol in beer.

  7. Detection of synthetic corticosteroids in bovine urine by chemiluminescence high-performance liquid chromatography.

    Science.gov (United States)

    Vázquez, B I; Feás, X; Lolo, M; Fente, C A; Franco, C M; Cepeda, A

    2005-01-01

    The development of a black market of chemical cocktails for illegal growth promotion in food-producing animals includes substances that are potentially dangerous for human health, such as synthetic corticosteroids. The potential presence of these residues in food makes it necessary to develop rapid and sensitive analytical methodologies to detect such substances, preferably in live animals before they arrive at the market. A chemiluminescence (CL) detection method for the determination of four synthetic corticosteroids (prednisolone, betamethasone, dexamethasone and flumethasone) in bovine urine has been developed. The proposed system, which does not need any derivatization procedure, offers an easy method well suited for routine research. Urine samples were homogenized with methanol:water (50:50, v/v) and centrifuged. The upper layer was collected and Strata X cartridges were used for cleaning up. The purified residues were evaporated to dryness and then redissolved in the mobile phase. Analysis of the extracts was performed using high-performance liquid chromatography with chemiluminescence detection, employing luminol as the CL reagent. The recovery curves, obtained at four spiking levels (different for each corticosteroid), showed that recoveries of at least 70% could be obtained for urine. The chemiluminescence detection procedure afforded satisfactory results with respect to sensitivity and the LOD and LOQ, taken as the first point of the regression curve, ranged from 4 ppb to 65 ppb. The maximum mean RSD was below 13% and below 15% for intra- and inter-day assay, respectively, in all cases.

  8. Optimised determination of clobazam in human plasma with extraction and high-performance liquid chromatography analysis.

    Science.gov (United States)

    Bolner, A; Tagliaro, F; Lomeo, A

    2001-01-05

    The analysis of clobazam by high-performance liquid chromatography and UV detection is described herein. After adding an internal standard, 600 microl of plasma were extracted under basic conditions onto disposable cartridges packed with celite. The organic extract was then evaporated to dryness and the residue reconstituted in 200 microl of mobile phase. A 20 microl aliquot was injected into chromatograph. The HPLC system was equipped with an Ultrasphere C8 analytical column coupled with an UV detector set at 235 nm. The mobile phase was an acetate buffer 20 mM, pH 5.5, containing acetonitrile and triethylamine 70:30:0.01 (v/v); the flow-rate was 1.8 ml/min. Using this method, clobazam can be detected with a sensitivity limit of 6 ng/ml and the RSD% intra- and inter-assay were lower than 5%. For its ruggedness and reliability, the proposed method is particularly suitable for therapeutic drug monitoring in epilepsy.

  9. Simultaneous determination of 11 preservatives in cosmetics by high-performance liquid chromatography.

    Science.gov (United States)

    Aoyama, Airin; Doi, Takahiro; Tagami, Takaomi; Kajimura, Keiji

    2014-10-01

    Preservatives prevent the growth of microorganisms in foods, pharmaceuticals and cosmetics. There exist numerous restrictions regarding the maximum allowable levels of preservatives in cosmetics. We analyzed 11 regulated preservatives in commercial cosmetics and manufacturers need to analyze their products for quality control purposes. However, methods used in previous studies to date have been inadequate for use by public institutions and manufacturers. Therefore, an effective, scalable method for the analysis of preservatives in cosmetics is required. We developed a novel method for the simultaneous determination of 11 regulated preservatives in cosmetics by high-performance liquid chromatography (HPLC). We applied the samples to a C18 column in a simple mobile phase (5 mmol/L ammonium formate solution and acetonitrile) with gradient elution at a flow rate of 1.0 mL/min at a single wavelength (230 nm). The correlation coefficients of the calibration curves were >0.997. The percent recoveries were 92.8-111.9% and the relative standard deviations were preservatives was >1.9. Because of the simple conditions for isolation and complete separation, the HPLC method can be effectively applied to the analysis of preservatives in commercially retailed cosmetics.

  10. MODELING VAPOR LIQUID EQUILIBRIUM OF IONIC LIQUIDS plus GAS BINARY SYSTEMS AT HIGH PRESSURE WITH CUBIC EQUATIONS OF STATE

    OpenAIRE

    Freitas, ACD; Cunico, LP; M. Aznar; Guirardello,R.

    2013-01-01

    Ionic liquids (IL) have been described as novel environmentally benign solvents because of their remarkable characteristics. Numerous applications of these solvents continue to grow at an exponential rate. In this work, high pressure vapor liquid equilibria for 17 different IL + gas binary systems were modeled at different temperatures with Peng-Robinson (PR) and Soave-Redlich-Kwong (SRK) equations of state, combined with the van der Waals mixing rule with two binary interaction parameters (v...

  11. Detection of argan oil adulteration with vegetable oils by high-performance liquid chromatography-evaporative light scattering detection.

    Science.gov (United States)

    Salghi, Rachid; Armbruster, Wolfgang; Schwack, Wolfgang

    2014-06-15

    Triacylglycerol profiles were selected as indicator of adulteration of argan oils to carry out a rapid screening of samples for the evaluation of authenticity. Triacylglycerols were separated by high-performance liquid chromatography-evaporative light scattering detection. Different peak area ratios were defined to sensitively detect adulteration of argan oil with vegetable oils such as sunflower, soy bean, and olive oil up to the level of 5%. Based on four reference argan oils, mean limits of detection and quantitation were calculated to approximately 0.4% and 1.3%, respectively. Additionally, 19 more argan oil reference samples were analysed by high-performance liquid chromatography-refractive index detection, resulting in highly comparative results. The overall strategy demonstrated a good applicability in practise, and hence a high potential to be transferred to routine laboratories.

  12. Mixed-mode chromatography integrated with high-performance liquid chromatography for protein analysis and separation: Using bovine serum albumin and lysozyme as the model target.

    Science.gov (United States)

    Xia, Hai-Feng; Don, Bin-Bin; Zheng, Meng-Jie

    2016-05-01

    A type of mixed-mode chromatography was integrated with high-performance liquid chromatography for protein analysis and separation. The chromatographic behavior was tested using bovine serum albumin and lysozyme as model proteins. For the mixed-mode column, the silica beads were activated with γ-(2,3-epoxypropoxy)-propytrimethoxysilane and coupled with 4-mercaptopyridine as the functional ligand. The effects of pH, salt, and the organic solvent conditions of the mobile phase on the retention behavior were studied, which provided valuable clues for separation strategy. When eluted with a suitable pH gradient, salt concentration gradient, and acetonitrile content gradient, the separation behavior of bovine serum albumin and lysozyme could be controlled by altering the conditions of the mobile phase. The results indicated this type of chromatography might be a useful method for protein analysis and separation.

  13. Chiral stationary phases based on chitosan bis(methylphenylcarbamate)-(isobutyrylamide) for high-performance liquid chromatography.

    Science.gov (United States)

    Tang, Sheng; Bin, Qin; Chen, Wei; Bai, Zheng-Wu; Huang, Shao-Hua

    2016-04-01

    A series of chitosan bis(methylphenylcarbamate)-(isobutyrylamide) derivatives were synthesized by carbamylating chitosan isobutyrylamide with different methylphenyl isocyanates. Then the prepared chitosan derivatives were coated onto 3-aminopropyl silica particles, resulting in a series of new chiral stationary phases (CSPs) for high-performance liquid chromatography. It was observed that the chiral recognition abilities of these coated-type CSPs depended very much on the substituents on the phenyl moieties of the chitosan derivatives, the eluent composition, as well as the structure of racemates. As a typical example, the eluent tolerance of the prepared CSP with the best enantioseparation ability was investigated in detail, and the results revealed that the CSP exhibited extraordinary solvent tolerance and could still work without significant loss in enantioseparation capability after being flushed with chloroform (100%), ethyl acetate (100%) and even THF/n-hexane (70/30, v/v), while the traditional coated-type CSPs based on the cellulose and amylose derivatives, such as cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) and amylose tris(3,5-dimethylphenylcarbamate) (ADMPC), might be dissolved or highly swollen in these eluents. Therefore, the application of the resultant CSPs could address the problem of the dissolution and high swelling of traditional coated-type CSPs in some unusual eluents, broadening the possibility of eluent choice. In addition, a comparison of the prepared CSPs with the well known CDMPC- and ADMPC- based CSPs concerning the chiral recognition ability was also made. Separation performances achieved on the as-prepared CSPs in different eluents were found to be even superior to CDMPC- and ADMPC-based CSPs for the tested chiral compounds. In summary, we could safely draw the conclusion that the CSPs derived from chitosan isobutyrylamide derivatives were capable of excellent chiral recognition ability, and meanwhile possessed satisfactory

  14. Robust naphthyl methacrylate monolithic column for high performance liquid chromatography of a wide range of solutes.

    Science.gov (United States)

    Jonnada, Murthy; El Rassi, Ziad

    2015-08-28

    An organic monolithic column based on the co-polymerization of 2-naphthyl methacrylate (NAPM) as the functional monomer and trimethylolpropane trimethacrylate (TRIM) as the crosslinker was introduced for high performance reversed-phase liquid chromatography (RPC). The co-polymerization was performed in situ in a stainless steel column of 4.6mm i.d. in the presence of a ternary porogen consisting of 1-dodecanol and cyclohexanol. This monolithic column (referred to as naphthyl methacrylate monolithic column or NMM column) showed high mechanical stability at relatively high mobile phase flow velocity indicating that the column has excellent hydrodynamic characteristics. To characterize the NMM column, different probe molecules including alkyl benzenes, and aniline, benzene, toluene and phenol derivatives were chromatographed on the column and the results in terms of k, selectivity and plate counts were compared to those obtained on an octadecyl silica (ODS) column in order to assess the presence of π-π and hydrophobic interactions on the NMM column under otherwise the same elution conditions. The NMM column offered additional π-π interactions with aromatic molecules in addition to hydrophobic interactions under RPC elution conditions. Run-to-run and column-to-column reproducibility of solute k values were evaluated, and percent relative standard deviation of column using shallow (30min at 1.0mL/min), steep (10min at 1.0mL/min) and ultra steep (1min at 3.0mL/min) linear gradient elution at increasing ACN concentration in the mobile phase using a 10cm×4.6mm i.d. column in case of shallow and steep linear gradients and a 3cm×4.6mm i.d. column for ultra steep linear gradient.

  15. Determination of nucleosides in Cordyceps sinensis and Ganoderma lucidum by high performance liquid chromatography method

    Science.gov (United States)

    Khan, Masood Shah; Parveen, Rabea; Mishra, Kshipra; Tulsawani, Rajkumar; Ahmad, Sayeed

    2015-01-01

    Background: Nucleosides are supportive in the regulation and modulation of various physiological processes in body, they acts as precursors in nucleic acid synthesis, enhance immune response, help in absorption of iron and influence the metabolism of fatty acids. Cordyceps sinensis and Ganoderma lucidum are well-known for its use in traditional medicine of China, Nepal and India. They are rich in nucleosides such as adenine, adenosine, cordycepin, etc. Hence, a simple, economic and accurate high-performance liquid chromatography (HPLC) analytical method was proposed for determination of adenine and adenosine for the quality control of plants. Materials and Methods: Chromatographic experiments were conducted on YL9100 HPLC system (South Korea). Reversed-phase chromatography was performed on a C18 column with methanol and dihydrogen phosphate as the mobile phase in isocratic elution method at a flow rate of 1.0 mL/min. Detection was carried out at 254 nm, which gives a sharp peak of adenine and adenosine at a retention time of 6.53 ± 0.02 min and 12.41 ± 0.02, respectively. Results and Discussion: Linear regression analysis data for the calibration plot showed a good linear relationship between response and concentration in the range of 25–200 µg/mL for adenosine and 100–800 µg/mL for adenine with regression coefficient of 0.999 and 0.996, respectively. The adenine was found 0.16% and 0.71% w/w in G. lucidum and in C. sinensis, respectively, and adenosine was found to be 0.14% w/w in G. lucidum whereas absent in C. sinensis. Conclusion: The developed HPLC method for the quantification of adenosine and adenine can be used for the quality control and standardization of crude drug and for the different herbal formulations, in which adenine and adenosine are present as major constituents. The wide linearity range, sensitivity, accuracy, and simple mobile phase imply the method is suitable for routine quantification of adenosine and adenine with high precision and

  16. Determination of nucleosides in Cordyceps sinensis and Ganoderma lucidum by high performance liquid chromatography method

    Directory of Open Access Journals (Sweden)

    Masood Shah Khan

    2015-01-01

    Full Text Available Background: Nucleosides are supportive in the regulation and modulation of various physiological processes in body, they acts as precursors in nucleic acid synthesis, enhance immune response, help in absorption of iron and influence the metabolism of fatty acids. Cordyceps sinensis and Ganoderma lucidum are well-known for its use in traditional medicine of China, Nepal and India. They are rich in nucleosides such as adenine, adenosine, cordycepin, etc. Hence, a simple, economic and accurate high-performance liquid chromatography (HPLC analytical method was proposed for determination of adenine and adenosine for the quality control of plants. Materials and Methods: Chromatographic experiments were conducted on YL9100 HPLC system (South Korea. Reversed-phase chromatography was performed on a C18 column with methanol and dihydrogen phosphate as the mobile phase in isocratic elution method at a flow rate of 1.0 mL/min. Detection was carried out at 254 nm, which gives a sharp peak of adenine and adenosine at a retention time of 6.53 ± 0.02 min and 12.41 ± 0.02, respectively. Results and Discussion: Linear regression analysis data for the calibration plot showed a good linear relationship between response and concentration in the range of 25–200 µg/mL for adenosine and 100–800 µg/mL for adenine with regression coefficient of 0.999 and 0.996, respectively. The adenine was found 0.16% and 0.71% w/w in G. lucidum and in C. sinensis, respectively, and adenosine was found to be 0.14% w/w in G. lucidum whereas absent in C. sinensis. Conclusion: The developed HPLC method for the quantification of adenosine and adenine can be used for the quality control and standardization of crude drug and for the different herbal formulations, in which adenine and adenosine are present as major constituents. The wide linearity range, sensitivity, accuracy, and simple mobile phase imply the method is suitable for routine quantification of adenosine and adenine with

  17. Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

    Science.gov (United States)

    Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

    2016-12-01

    Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL(-1), respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%.

  18. Determination of nicotine and N-nitrosamines in house dust by pressurized liquid extraction and comprehensive gas chromatography--nitrogen chemiluminiscence detection.

    Science.gov (United States)

    Ramírez, Noelia; Ozel, Mustafa Z; Lewis, Alastair C; Marcé, Rosa M; Borrull, Francesc; Hamilton, Jacqueline F

    2012-01-06

    A novel, highly selective method for the determination of nicotine, N-nitrosamines and tobacco-specific nitrosamines (TSNAs) in indoor dust samples is presented in this study. Samples were extracted by in-cell clean-up pressurized liquid extraction (PLE) that allows high extraction efficiency with moderate consumption of organic solvents. The extracts were analyzed by comprehensive gas chromatography and detected with a nitrogen chemiluminiscence detector (GC×GC-NCD) that provided enhanced selectivity and sensitivity for organic nitrogen containing compounds. Method validation showed good linearity, repeatability and reproducibility (%RSD<8%). Recovery was higher than 80% for most target compounds and limits of detection lower than 16 ng g(-1). The method was used for the determination of the nitrosamine target compounds in house dust samples from both smoking and non-smoking households. All the analytes were found in the samples, nicotine being the most abundant compound in smokers' dust and one of the most abundant in non-smokers' dust. To our knowledge this is the first time that volatile N-nitrosamines and TSNAs have been determined in indoor dust samples. The results demonstrate the presence of these highly carcinogenic compounds in house dust, with inherent human exposure through inhalation and/or involuntary ingestion of house dust.

  19. Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid-liquid microextraction as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Li, Nai; Cao, Xueli

    2015-05-01

    In-situ ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) method was developed as a pretreatment method for the detection of six chlorophenols (CPs) in honey samples. The hydrophobic ionic liquid [C4MIM][NTf2], formed in-situ by the hydrophilic ionic liquid [C4MIM][BF4] and the ion exchange reagent LiNTf2 was used as the microextractant solvent of CPs from honey sample. Then the enriched analytes were back-extracted into 40 μL of 0.14 M NaOH solution and finally subjected to analysis by high-performance liquid chromatography. The method showed low limit of detection of CPs, 0.8-3.2 μg/L and high enrichment factor, 34-65 with the recoveries range from 91.60% to 114.33%. The method is simple, rapid, environmentally friendly and with high extraction efficiency.

  20. A new automated method to analyze urinary 8-hydroxydeoxyguanosine by a high-performance liquid chromatography-electrochemical detector system.

    Science.gov (United States)

    Kasai, Hiroshi

    2003-06-01

    A new method was developed to analyze urinary 8-hydroxydeoxyguanosine (8-OH-dG) by high-performance liquid chromatography (HPLC) coupled to an electrochemical detector (ECD). This method is unique because (i) urine is first fractionated by anion exchange chromatography (polystyrene-type resin with quaternary ammonium group, sulfate form) before analysis by reverse phase chromatography; and (ii) the 8-OH-dG fraction in the first HPLC is precisely and automatically collected based on the added ribonucleoside 8-hydroxyguanosine marker peak, which elutes 4-5 min earlier. Up to 1,000 human urine samples can be continuously analyzed with high accuracy within a few months. This method will be useful for studies in radiotherapy, molecular epidemiology, risk assessment, and health promotion.

  1. Ultra-high-performance liquid chromatography profiling method for chemical screening of proanthocyanidins in Czech hops.

    Science.gov (United States)

    Olšovská, J; Kameník, Z; Čejka, P; Jurková, M; Mikyška, A

    2013-11-15

    Hops represent an important natural source of bioactive polyphenols, particularly proanthocyanidins, which can contribute to prevention of several civilization diseases, owing to their antioxidant and radical scavenging activity. We have developed a high-throughput ultra-high-performance liquid chromatography time-of-flight mass spectrometry profiling method, which can be used for monitoring of bioactive proanthocyanidins in hops. The method was applied for analysis of hops of four Czech varieties (Saaz, Sladek, Preminat and Agnus) from the 2011 crop (9 localities, 11 samples) and the 2012 crop (24 localities, 40 samples). Hop samples were extracted by acetone and the analytes were separated on the Acquity UPLC BEH Shield RP18 column. Partial validation of the method revealed a satisfactory intra-day repeatability of the method for retention times (relative standard deviation within 1.39%) as well as areas under the peaks (within 9.89%). Experimental data were evaluated using principal component analysis and cluster analysis. Significant amounts of di-, tri- and tetramer proanthocyanidins consisting of (epi)catechin and (epi)gallocatechin were found in the hop samples. The dependence of the proantocyanidin composition on both the variety and the growing locality was observed. Specifically, the traditional Saaz variety contained more frequently oligomers formed by (epi)catechin units only, whereas the varieties Premiant and Agnus produced oligomers consisting of (epi)catechin as well as (epi)gallocatechin units. The relative abundance of proanthocyanidins in studied hop varieties from the two crops, 2011 and 2012, did correspond to each other. In the further perspective, the method may also be used for prediction of qualitative marks or authenticity verification of hops.

  2. Quantification of free formaldehyde in carrageenan and processed Eucheuma seaweed using high-performance liquid chromatography.

    Science.gov (United States)

    Hornshøj, Bettina Høj; Kobbelgaard, Sara; Blakemore, William R; Stapelfeldt, Henrik; Bixler, Harris J; Klinger, Markus

    2015-01-01

    In 2010 the European Commission placed a limit on the amount of free formaldehyde in carrageenan and processed Eucheuma seaweed (PES) of 5 mg kg(-1). Formaldehyde is not used in carrageenan and PES processing and accordingly one would not expect free formaldehyde to be present in carrageenan and PES. However, surprisingly high levels up to 10 mg kg(-1) have been found using the generally accepted AOAC and Hach tests. These findings are, per proposed reaction pathways, likely due to the formation of formaldehyde when sulphated galactose, the backbone of carrageenan, is hydrolysed with the strong acid used in these conventional tests. In order to minimise the risk of false-positives, which may lead to regulatory non-compliance, a new high-performance liquid chromatography (HPLC) method has been developed. Initially, carrageenan or PES is extracted with 2-propanol and subsequently reacted with 2,4-dinitrophenylhydrazine (DNPH) to form the chromophore formaldehyde-DNPH, which is finally quantified by reversed-phase HPLC with ultraviolet light detection at 355 nm. This method has been found to have a limit of detection of 0.05 mg kg(-1) and a limit of quantification of 0.2 mg kg(-1). Recoveries from samples spiked with known quantities of formaldehyde were 95-107%. Using this more specific technique, 20 samples of carrageenan and PES were tested for formaldehyde. Only one sample had a detectable content of formaldehyde (0.40 mg kg(-1)), thus demonstrating that the formaldehyde content of commercial carrageenan and PES products are well below the European Commission maximum limit of 5 mg kg(-1).

  3. Determination of testosterone propionate residues in fish and shrimp by high pressure liquid chromatography-tandem mass spectrometry with isotope dilution%同位素稀释高压液相色谱-串联质谱法测定鱼虾中丙酸睾酮残留量

    Institute of Scientific and Technical Information of China (English)

    田良良; 林洪; 曹立民; 蔡友琼; 王建华; 黄冬梅; 史永富

    2014-01-01

    Objective A rapid, specific and highly sensitive method for the determination of testosterone propio-nateresidue in fish and shrimp was developed using high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Homogenized tissue samples which were added with nandrolone-D3 were extracted by tert-butyl ether under ultrasonication and cleaned up with freezing and high-speed centrifugation. The target compounds were separated on Eclipse Plus C18 (100 mm×2.1 mm, 3μm) using acetonitrile-0.1%formic acid as mobile phase at a flow rate of 0.3 mL/min, and detected qualitatively and quantitatively in selected reaction monitoring(SRM) under posi-tive mode. Results The linearity ranged from 0.5 to 100 ng/mL and correlation coefficient was 0.9989. The limit of quantitation (LOQ) was 0.5μg/kg. At the spiked levels of 0.5, 1.0, 2.0μg/kg and 10.0μg/kg, the average recoveries ranged from 71.2% to 104.5%. The relative standard deviations were between 2.26% and 5.65%. Conclusion The method is simple, sensitive and accurate for detecting the testosterone propionate in aquatic products.%目的:采用高压液相色谱-串联质谱(high pressure liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)快速检测鱼虾等水产品中丙酸睾酮残留。方法向捣碎匀浆后的样品中加入内标诺龙-D3混匀后,叔丁基甲醚超声提取,-80℃冷冻30 min后12000 r/min离心净化。以Eclipse Plus C18为色谱分离柱,以乙腈-0.1%甲酸水溶液为流动相,流速为0.3 mL/min,采用三重四极杆质谱在正离子模式下进行选择反应离子监测。结果丙酸睾酮在0.5~100 ng/mL范围内呈线性关系,相关系数为0.9989;方法定量限为0.5μg/kg。当添加水平为0.5~10.0μg/kg时,平均回收率为71.2%~104.5%,相对标准偏差为2.26%~5.65%。结论该方法操作简单、快速、灵敏度高,适用于快速检测水产品中丙酸睾酮的残留量。

  4. Analysis of sup 99m Tc-labeled radiopharmaceuticals by high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Muto, Toshio (Tokyo Metropolitan Isotope Research Center (Japan))

    1990-02-01

    High-performance liquid chromatography (HPLC) equiped with on line radiometric and optical detectors (i.e. radio-HPLC) have been applied to the radiochemical analysis of commonly-used {sup 99m}Tc-radio pharma ceuticals with a view point to check the radiochemical purities of the compounds. Chromatographic conditions were determined by examination of the types of column, mobile phase and pH. An aqueous size-exclusion (Shim-pack Diol-300) and reversed-phase column (Zorbax-ODS) were found to be suitable for {sup 99m}Tc-HSA and the other {sup 99m}Tc-agents, respectively. The analysis of low molecular weight {sup 99m}Tc-agents (e.g. {sup 99m}Tc-DTPA, {sup 99m}Tc-DMSA, {sup 99m}Tc-pyrophosphate, {sup 99m}Tc-phytic acid, {sup 99m}Tc-MDS, {sup 99m}Tc-HMDP) were done by reversed-phaseion pairing chromatography using a optimized mobile phase consisted on a mixture of 50 mM phosphate buffer (pH 7.0) and 2 mM TBA (tetra nbutyl) ammonium hydroxide in 30 % methanol. The mobile phases for analysis of medium molecular weight {sup 99m}Tc-HSA were consisted of a mixture of 50 mM phosphate buffer (ph 7.0) in 30 % methanol, and a mixtures of 1 % SDS (sodium dodecyl sulfonate) in Tris buffer (pH. 7.0), respectively. It was apparent from the radio-chromatograms obtained from these chromatographic conditions, that impurity of {sup 99m}TcO{sub 4} was observed in {sup 99m}Tc-pyrophosphate, {sup 99m}Tc-phytic acid, {sup 99m}Tc-MDP, {sup 99m}Tc-HMDP, and impurities of {sup 99m}Tc-labeled species and {sup 99m}TcO{sub 4}, were observed in {sup 99m}Tc-HIDA, {sup 99m}Tc-HIDA, {sup 99m}Tc-HSA. The radiochemical impurities of the {sup 99m}Tc-radiopharmaceuticals were ranged between 90 and 100 %. From these results, radio-HPLC has been shown to be suitable method for analysis of {sup 99m}Tc-radiopharmaceuticals, with rapidity and excellent precision. (author).

  5. Comparative analysis of steroidal saponins in four Dioscoreae herbs by high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Guo, Long; Zeng, Su-Ling; Zhang, Yu; Li, Ping; Liu, E-Hu

    2016-01-01

    Steroidal saponins, which exhibit multiple pharmacological effects, are the major bioactive constituents in herbal medicines from Dioscoreae species. In this study, a sensitive method based on high performance liquid chromatography-mass spectrometry (HPLC-MS) was established and validated for qualitative and quantitative analysis of steroidal saponins in four Dioscoreae herbs including Dioscoreae Nipponica Rhizome (DNR) and Dioscoreae Hypoglaucae Rhizome (DHR), Dioscoreae Spongiosae Rhizome (DSR) and Dioscoreae Rhizome (DR). A total of eleven steroidal saponins were identified by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF/MS). Furthermore, seven major steroidal saponins was simultaneous quantified using a high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ/MS). The qualitative and quantitative analysis results indicated that the chemical composition of DNR, DHR and DSR samples exhibited a high level of global similarity, while the ingredients in DR varied greatly from the other three herbs. Moreover, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were performed to compare and discriminate the Dioscoreae herbs based on the quantitative data. The results demonstrated the qualitative and quantitative analysis of steroidal saponins based on HPLC-MS is a feasible method for quality control of Dioscoreae herbs.

  6. Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for determination of benzoate and sorbate in yogurt drinks and method optimization by central composite design.

    Science.gov (United States)

    Kamankesh, Marzieh; Mohammadi, Abdorreza; Tehrani, Zohreh Modarres; Ferdowsi, Roohallah; Hosseini, Hedayat

    2013-05-15

    A new method based on dispersive liquid-liquid microextraction (DLLME) followed by high-performance liquid chromatography (HPLC) for determination of benzoate and sorbate salts in yogurt drinks was developed. The effective parameters in DLLME process, including volume of extraction and disperser solvents, pH and salt effect, were optimized using response surface methodology (RSM) based on central composite design. The yogurt drink samples were extracted using NaOH and Carrez solutions (potassium hexaferrocyanide and zinc acetate) were used for sedimentation of proteins. For DLLME, a mixture of extraction solvent (1-octanol) and disperser solvent (ethanol) was rapidly injected into the sample solution by syringe and cloudy solution is formed. Subsequently, the upper 1-octanol layer was analyzed by HPLC. The detection limits for benzoate and sorbate were 0.06 ng mL(-1) and 0.15 ng mL(-1), respectively. The relative standard deviations (RSD) for seven analyses were 4.96% for benzoate and 4.58% for sorbate. The proposed method demonstrated good linearity and high enrichment factor. A clean separation and good chromatogram is readily achieved without the presence of matrix interference. A comparison of this method with previous methods demonstrated that the proposed method is an accurate, rapid and reliable sample-pretreatment method that gives very good enrichment factors and detection limits for extracting and determining sorbate and benzoate in yogurt drink samples.

  7. Determination of six pyrethroid insecticides in fruit juice samples using dispersive liquid-liquid microextraction combined with high performance liquid chromatography.

    Science.gov (United States)

    Boonchiangma, Suthasinee; Ngeontae, Wittaya; Srijaranai, Supalax

    2012-01-15

    Dispersive liquid-liquid microextraction (DLLME) coupled to high performance liquid chromatography (HPLC) with UV detection was applied for the determination of six pyrethroids (tetramethrin, fenpropathrin, cypermethrin, deltamethrin, fenvalerate and permethrin) in various fruit juices including apple, red grape, orange, kiwi, passion fruit, pomegranate and guava juice. Six pyrethroids were separated within 30 min using a Waters Atlantis T3 column under an isocratic elution of acetonitrile-water (72:28). The parameters affecting extraction efficiency of the DLLME method such as type of disperser and extraction solvent, volume of disperser and extraction solvent and centrifugation time were investigated. Under the optimum conditions, 5.00 mL of sample solution, 300 μL of chloroform as extraction solvent and 1.25 mL of methanol as dispersive solvent gave high enrichment factor in the range of 62-84. Good linearity was obtained from 2 to 1,500 μg/L (r(2)>0.995). The mean recoveries of the pyrethroids evaluated by fortification of real samples were in the range of 84-94%. The limits of detection ranging from 2 to 5 μg/L are sufficient to analyze pyrethroid residues at the maximum residue limits (MRLs) established by the European Union (EU) in fruit juices. The proposed method can be applied to direct determination of pyrethroid residues in fruit juices.

  8. Vortex-assisted low density solvent based demulsified dispersive liquid-liquid microextraction and high-performance liquid chromatography for the determination of organophosphorus pesticides in water samples.

    Science.gov (United States)

    Seebunrueng, Ketsarin; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2014-05-01

    A simple, rapid, effective and eco-friendly preconcentration method, vortex-assisted low density solvent based solvent demulsified dispersive liquid-liquid microextraction (VLDS-SD-DLLME), followed by high performance liquid chromatography-diode array detector (HPLC-DAD) analysis, has been developed for the first time for the determination of four organophosphorus pesticides (OPPs) (e.g., azinphos-methyl, parathion-methyl, fenitrothion and diazinon) in environmental water samples. In this preconcentration procedure, an emulsion was obtained after the mixture of extraction solvent (1-dodecanol) and dispersive solvent (acetonitrile, ACN) was injected rapidly into 10 mL of the sample solution. The vortex agitator aided the dispersion of the extraction solvent into the sample solution. After the formation of an emulsion, the demulsifier (ACN) was added, resulting in the rapid separation of the mixture into two phases without centrifugation. Under optimal conditions, the proposed method provided high extraction efficiency (90-99%), good linearity range (0.5-500 ng mL(-1)), low limits of detection (0.25-1 ng mL(-1)) and good repeatability and recoveries were obtained.

  9. Enantiomeric high-performance liquid chromatography resolution and absolute configuration of 6β-benzoyloxy-3α-tropanol.

    Science.gov (United States)

    Muñoz, Marcelo A; González, Natalia; Joseph-Nathan, Pedro

    2016-07-01

    The absolute configuration of the naturally occurring isomers of 6β-benzoyloxy-3α-tropanol (1) has been established by the combined use of chiral high-performance liquid chromatography with electronic circular dichroism detection and optical rotation detection. For this purpose (±)-1, prepared in two steps from racemic 6-hydroxytropinone (4), was subjected to chiral high-performance liquid chromatography with electronic circular dichroism and optical rotation detection allowing the online measurement of both chiroptical properties for each enantiomer, which in turn were compared with the corresponding values obtained from density functional theory calculations. In an independent approach, preparative high-performance liquid chromatography separation using an automatic fraction collector, yielded an enantiopure sample of OR (+)-1 whose vibrational circular dichroism spectrum allowed its absolute configuration assignment when the bands in the 1100-950 cm(-1) region were compared with those of the enantiomers of esters derived from 3α,6β-tropanediol. In addition, an enantiomerically enriched sample of 4, instead of OR (±)-4, was used for the same transformation sequence, whose high-performance liquid chromatography follow-up allowed their spectroscopic correlation. All evidences lead to the OR (+)-(1S,3R,5S,6R) and OR (-)-(1R,3S,5R,6S) absolute configurations, from where it follows that samples of 1 isolated from Knightia strobilina and Erythroxylum zambesiacum have the OR (+)-(1S,3R,5S,6R) absolute configuration, while the sample obtained from E. rotundifolium has the OR (-)-(1R,3S,5R,6S) absolute configuration.

  10. Investigation of retention and chiral recognition mechanism using quantitative structure-enantioselectivity retention relationship in high performance liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    CHEN, Hui; LU, Xian-Yu; GAO, Ru-Yu; HUANG, Jun-Min; YANG, Hua-Zheng; WANG, Qin-Sun

    2000-01-01

    The enantiomers of a series of fourteen O-ethyl O-(substituted) phenyl N-isopropyl-phosphoroamidothioates have been separated by high performance liquid chromatography (HPLC) on the Pirkde-type chiral stationary phase. Seven molecular descriptors were lculated and four .significant descriptors were chosen to correlate against the experimental Ink′ values in order to form thequantitative structure-enantioselectivity retention relationships (QSERRs). Through the QSERRs, the retention and enantioselectivity meehanism were examined.

  11. Protective properties of wine products and the role of high performance liquid chromatography in the study of these properties

    Science.gov (United States)

    Ulyanova, E. V.; Larionov, O. G.; Revina, A. A.; Andrievskaya, D. V.; Urusova, L. M.; Fenin, A. A.

    2013-12-01

    Data on the biologically active substances present in wines and wine products, the methods of their determination, and changes under chemical, radiation and other types of action are generalized. The role of high performance liquid chromatography in the studies of the protective properties of wines is demonstrated. Particular attention is devoted to problems of counterfeiting of wine products and the possibility to reveal it by using amperometric determination of the antioxidant activity. The bibliography includes 117 references.

  12. Isolation of lignans glycosides from Alibertia sessilis (Vell.) K. Schum. (Rubiaceae) by preparative high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Silva, V.C. da; Bolzani, V. da S.; Lopes, M.N. [UNESP, Araraquara, SP (Brazil). Inst. de Quimica. Dept. de Quimica Organica; Silva, G.H. [Universidade Federal de Sergipe, Aracaju, SE (Brazil). Dept. de Quimica]. E-mail: mnlopes@iq.unesp.br

    2006-10-15

    Enantiomeric aglycone lignans contained in a mixture were separated from a fraction of the extract of the stems of Alibertia sessilis (Vell.) K. Schum. (Rubiaceae) by preparative high-performance liquid chromatography. An efficient and fast separation can be achieved with methanol-water (30:70, v/v). Their structures were identified as (+)-lyoniresinol 3{alpha}-O-{beta}-glucopyranoside and (-)-lyoniresinol 3{alpha}-O-{beta}-glucopyranoside, being reported for the first time in Rubiaceae. (author)

  13. Determination of Sudan Residues in Sausage by Matrix Solid-Phase Dispersion and High-Performance Liquid Chromatography.

    Science.gov (United States)

    Zhai, Yujuan; Cheng, Jianhua

    2015-09-01

    A method based on matrix solid-phase dispersion and high-performance liquid chromatography was applied to the determination of four Sudan red residues in sausage. The proposed method required only 0.5 g sample. The neutral alumina was used as the dispersant sorbent while n-hexane containing 10% (v/v) acetone was used as the eluting solvent. The recoveries in samples ranged from 76.4 to 111.0% and relative standard deviations were sausage.

  14. Simultaneous determination of 20 food additives by high performance liquid chromatography with photo-diode array detector

    Institute of Scientific and Technical Information of China (English)

    Kang Ma; Ya Nan Yang; Xiao Xiong Jiang; Min Zhao; Ye Qiang Cai

    2012-01-01

    An efficient and accurate analytical method was developed for the simultaneous determination of 20 synthetic food additives,including three sweeteners,seven food colorants,nine synthetic preservatives and caffeine,by high performance liquid chromatography (HPLC) with photodiode array detector (PDA).This method permits the detection of food additives at very low concentrations (0.005-0.150 μg/mL).The applicability was verified by the determination of food additives present in various foodstuffs.

  15. Rapid determination of quinolones in cosmetic products by ultra high performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Liu, Shao-Ying; Huang, Xi-Hui; Wang, Xiao-Fang; Jin, Quan; Zhu, Guo-Nian

    2014-05-01

    This study developed an improved analytical method for the simultaneous quantification of 13 quinolones in cosmetics by ultra high performance liquid chromatography combined with ESI triple quadrupole MS/MS under the multiple reaction monitoring mode. The analytes were extracted and purified by using an SPE cartridge. The limits of quantification ranged from 0.03 to 3.02 μg/kg. The precision for determining the quinolones was quinolones in real cosmetic samples.

  16. DETERMINATION OF GAMMA - AMINOBUTYRIC ACID BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    D. Qujeq

    1998-08-01

    Full Text Available Gamma-aminobutyric acid is the main inhibitory amino acid neurotransmitter in several areas of the brain. Measurement of gamma-aminobutyric acid in the brain will help elucidate its metabolic rote and diagnostic value. The liquid chromatography (LC system consisted of a delivery pump. Male rats (150-250g were used in this study. The brain was rapidly removed from decapitated animals. Trie chromatograms showed satisfactory resolution and symmetrical peak shapes, both with the standard and tissue extracts. the retention lime was 4.60 min. it was constant in repeated analyses and exactly the same for the standard and tissue samples.

  17. Ultra pressure liquid chromatography-negative electrospray ionization mass spectrometry determination of twelve halobenzoquinones at ng/L levels in drinking water.

    Science.gov (United States)

    Huang, Rongfu; Wang, Wei; Qian, Yichao; Boyd, Jessica M; Zhao, Yuli; Li, Xing-Fang

    2013-05-01

    We report here the characterization of twelve halobenzoquinones (HBQs) using electrospray ionization (ESI) high resolution quadrupole time-of-flight mass spectrometry. The high resolution negative ESI spectra of the twelve HBQs formed two parent ions, [M + H(+) + 2e(-)], and the radical M(-•). The intensities of these two parent ions are dependent on their chemical structures and on instrumental parameters such as the source temperature and flow rate. The characteristic ions of the HBQs were used to develop an ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. At the UPLC flow rate (400 μL/min) and under the optimized ESI conditions, eleven HBQs showed the stable and abundant transitions [M + H(+) + 2e(-)] → X(-) (X(-) representing Cl(-), Br(-), or I(-)), while dibromo-dimethyl-benzoquinone (DBDMBQ) showed only the transition of M(-•) → Br(-). The UPLC efficiently separates all HBQs including some HBQ isomers, while the MS/MS offers exquisite limits of detection (LODs) at subng/mL levels for all HBQs except DBDMBQ. Combined with solid phase extraction (SPE), the method LOD is down to ng/L. The results from analysis of authentic samples demonstrated that the SPE-UPLC-MS/MS method is reliable, fast, and sensitive for the identification and quantification of the twelve HBQs in drinking water.

  18. Identification, characterization, and high-performance liquid chromatography quantification of process-related impurities in vonoprazan fumarate.

    Science.gov (United States)

    Liu, Lei; Cao, Na; Ma, Xingling; Xiong, Kaihe; Sun, Lili; Zou, Qiaogen

    2016-04-01

    High-performance liquid chromatography analysis of vonoprazan fumarate, a novel proton pump inhibitor drug revealed six impurities. These were identified by liquid chromatography with mass spectrometry. Further, the structures of the impurities were confirmed by synthesis followed by characterization by mass spectrometry, NMR spectroscopy, and infrared spectroscopy. On the basis of these data and knowledge of the synthetic scheme of vonoprazan fumarate, the previously unknown impurity was identified as 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3-yl]-N-methyldimethylamine, which is a new compound. The possible mechanisms by which these impurities were formed were also discussed. A high-performance liquid chromatography method was optimized in order to separate, selectively detect, and quantify all process-related impurities of vonoprazan fumarate. The presented method has been validated in terms of linearity, limits of detection, and quantification, and response factors and, therefore, is highly suitable for routine analysis of vonoprazan fumarate related substances as well as stability studies.

  19. Speciation of arsenic using chelation solvent extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Cathum, Shamil J.; Obenauf, Alison; Punt, Monique [SAIC Canada, Ottawa, Ontario (Canada); Brown, Carl E. [Emergencies Engineering Technology Office, Environmental Technology Centre, Environment Canada, Ottawa, Ontario (Canada)

    2007-02-15

    Research interest in speciation of arsenic stems from its species dependent behavior in the environment and in living organisms. The complexity of the matrix to be analyzed and low concentrations of target arsenic species that may be labile or difficult to chromatogram, indicate that a suitable pre-treatment methodology is required. This study investigated the usefulness of chelation solvent extraction - high performance liquid chromatography (CSE-HPLC) for the speciation of arsenic in water. It involved reacting arsenic with the chelant known for its affinity towards arsenic, followed by extraction, separation, and identification of the arsenic-chelant-arsenic complex. Arsenic species having different physicochemical properties were investigated. Species, such as, As{sub 2}O{sub 3}, As{sub 3}O{sub 5}, KH{sub 2}AsO{sub 4}, Na{sub 2}HAsO{sub 4}, and NaAsO{sub 2}were detected as a group of closely eluted peaks with different retention times and spectral properties, whereas, the organic arsenic species CH {sub 3}Na {sub 2}AsO {sub 3}, o-arsanilic acid, roxarson and triphenyl arsine separated quite well on the EnviroseP-CM HPLC column. Key method parameters, such as, type of HPLC column, composition of mobile phase and organic solvents affecting peak resolution and sensitivity were optimized. Real environmental matrices contaminated with arsenic were analyzed under varying wavelengths ({lambda}{sub max} = 190, 210, 220, 234, 244, and 282 nm), with good precision. Different arsenic species were detected in these samples with excellent background and signal-to-noise ratios demonstrating the robustness of the method. The detection limit, reproducibility, selectivity, accuracy, and dynamic range of the calibration curves were evaluated. (Abstract Copyright [2007], Wiley Periodicals, Inc.)

  20. [Determination of aflatoxins in cashew by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Bi, Ruifeng; Fan, Zhixian; Fu, Meng

    2011-12-01

    A method for the determination of four aflatoxins in cashew using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The sample was extracted with methanol-water (8: 2, v/v) solution, followed by a cleanup procedure with Florisil column. The target compounds were eluted using 5 mL acetone-water-formic acid (96: 3.5:0.5, v/v/v) solution. The eluate was dried under N2, then dissolved in 1 mL methanol. Four aflatoxins were separated in MG C18 column (100 mm x 3.0 mm, 3 microm) adopting a gradient program within 15 min. A triple quadrupole mass spectrometry equipped with an electrospray ionization source operated in the positive ion mode was used to detect the aflatoxins. The good correlation coefficients (r2 > 0.997) of the four aflatoxins were obtained within their respective linear ranges. The limits of detection (S/N = 3) were between 0.009 microg/kg and 0.04 microg/kg, and the limits of quantification (S/N = 10) were between 0.03 microg/kg and 0.12 microg/kg. The recoveries were in a range of 63.0% -78.5% with the relative standard deviations (RSDs) varied from 2.8% to 9.1%. The validation results meet the requirements of trace assay. Matrix effects were estimated and the signal suppression/enhancement ranged from 88.8% to 99.4%. The results indicate that the developed method is simple, fast, accurate, and can be applied for the determination of fours aflatoxins in cashew.

  1. Determination of plasma lactic acid concentration and specific activity using high-performance liquid chromatography.

    Science.gov (United States)

    Bleiberg, B; Steinberg, J J; Katz, S D; Wexler, J; LeJemtel, T

    1991-08-23

    Assessment of lactate metabolism is of particular interest during exercise and in disease states such as diabetes, shock, and absorptive abnormalities of short-chain fatty acids by the colon. We describe an analytical method that introduces radio-active tracers and high-performance liquid chromatography (HPLC) to simultaneously analyze concentrations and specific activities (SAs) of plasma lactate. The HPLC conditions included separation on a reversed-phase column (octadecylsilane) and an isocratic buffer (30% acetonitrile in water). [3H]Acetate served as an internal standard. Lactate and acetate were extracted from plasma samples with diethyl ether following a pH adjustment to less than 1.0 and back-extracted into a hydrophilic phase with sodium carbonate (2 mM, pH greater than 10.0). Lactate is detected in the ultraviolet range (242 and 320 nm) by derivatization with alpha-bromoacetophenone. Control plasma samples were studied after an overnight fast for precision and analytical recovery. Calibration curves were linear in the range 0.18-6.0 mM (r = 0.92). The precision was 3% and the analytical recovery was 87%. The detection limit of the method was 36 pmol. Determination of lactate metabolism was performed in a patient with chronic congestive heart failure who was administered primed-continuous L-[U-14C]lactate (10 microCi bolus and 0.3 microCi/min continuously) during a 60-min rest period. Mean arterial lactate concentration and SA were 1.69 +/- 0.2 mM and 253.8 +/- 22 dpm/mumol, respectively. Systemic lactate turnover was 25.65 mumol/kg per min. Lactic acid systemic turnover, organ uptake and release rates can be accurately determined by isocratic HPLC.

  2. Characterization of Fumonisin A-Series by High-Resolution Liquid Chromatography-Orbitrap Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Tamura

    2014-08-01

    Full Text Available Fumonisin A-series (FAs in a reference material of corn sample that was naturally contaminated with fumonisins was characterized using high-resolution liquid chromatography-Orbitrap mass spectrometry (LC-Orbitap MS. Peaks for fumonisin B1 (FB1, fumonisin B2 (FB2, and fumonisin B3 (FB3, in addition to three peaks corresponding to unknown compounds I, II, and III, were detected in the chromatogram for the corn sample. Fragment ion analysis for FB1, FB2, and FB3 showed that while the ions formed at m/z values of 200–800 were similar to those formed by the cleavage of the tricarballylic acids and the hydroxyl groups, the fragmentation patterns at m/z values of 50–200 varied depending on the hydroxyl group locations in the compounds. Fragment ion analysis of compounds I–III revealed structural similarities to FBs, only differing by an additional C2H2O in the unknown compounds. Using these results and by comparing the product ion mass spectra of compound I with fumonisin A1 (FA1 synthesized from FB1 standards, compounds I–III were hypothesized to be N-acetyl analogs of FBs: fumonisins A1 (FA1, A2 (FA2, and A3 (FA3. The method for determining concentrations was validated with FA1, FB1, FB2, and FB3 standards and applied to analyze the reference material. The FB1, FB2, and FB3 analytical levels were within acceptance limits and the amount of FA1 in the material was ~15% of FB1 amount at 4.2 mg/kg.

  3. Enantiomeric Separations of Pyriproxyfen and its Six Chiral Metabolites by High-Performance Liquid Chromatography.

    Science.gov (United States)

    Zhang, Chuntao; Liu, Hui; Liu, Donghui; Wang, Liying; Gao, Jing; Zhou, Zhiqiang; Wang, Peng

    2016-03-01

    Pyriproxyfen is a chiral insecticide, and over 10 metabolites have been identified in the environment. In this work the separations of the enantiomers of pyriproxyfen and its six chiral metabolites were studied by high-performance liquid chromatography (HPLC). Both normal phase and reverse phase were applied using the chiral columns Chiralpak IA, Chiralpak IB, Chiralpak IC, Chiralcel OD, Chiralcel OD-RH, Chiralpak AY-H, Chiralpak AD-H, Chiracel OJ-H, (R,R)-Whelk-O 1, and Lux Cellulose-3. The effects of the chromatographic parameters such as mobile phase composition and temperature on the separations were investigated and the enantiomers were identified with an optical rotation detector. The enantiomers of these targets could obtain complete separations (resolution factor Rs > 1.5) on Chiralpak IA, Chiralpak IB, Chiralcel OD, Chiralpak AY-H, or Chiracel OJ-H under normal conditions. Chiralcel OJ-H showed the best chiral separation results with n-hexane as mobile phase and isopropanol (IPA) as modifier. The simultaneous enantiomeric separation of pyriproxyfen and four chiral metabolites was achieved on Chiralcel OJ-H under optimized condition: n-hexane/isopropanol = 80/20, 15°C, flow rate of 0.8 ml/min, and UV detection at 230 nm. The enantiomers of pyriproxyfen and the metabolites , , and obtained complete separations on Chiralpak IA, Chiralpak IC, and Lux Cellulose-3 under reverse phase using acetonitrile/water as the mobile phase. The retention factors (k) and selectivity factors (α) decreased with increasing temperature, and the separations were better under low temperature in most cases. The work is of significance for the investigation of the environmental behaviors of pyriproxyfen on an enantiomeric level.

  4. Simultaneous determination of multiple marker constituents in concentrated Gegen Tang granule by high performance liquid chromatography

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    Yip Yuekeung

    2007-06-01

    Full Text Available Abstract Background Concentrated Gegen Tang (GT granule is a widely available traditional Chinese medicinal product for the treatment of cold and flu. There was no reliable analytical method available for the quality assessment of GT granules. Methods An HPLC method with an Agilent Zorbax SB-Phenyl Stablebond column (250 × 4.6 mm, 5 μm was developed and validated. The mobile phase gradient was a mixture of 0.1% trifluoroacetic acid (TFA in acetonitrile (ACN and 0.1% TFA in water. The detection with a diode-array detector was set at 207, 230, 250 and 275 nm. Seven components, namely puerarin, daidzein, paeoniflorin, cinnamic acid, glycyrrhizin, ephedrine and pseudoephedrine were selected as marker compounds for the evaluation. Results The regression equations revealed good linear relationships (correlation coefficients: 0.9994–0.9998 between the peak areas and concentrations. The recovery was between 98.8% and 101.7% with good precision and accuracy. The quality of GT granule from four different manufacturers was evaluated with this newly developed method. Samples from four manufacturers showed similar profiles but contents of the detected markers varied significantly among manufacturers and batches. Conclusion A new method using high performance liquid chromatography (HPLC has been developed for simple and reliable quality control of commercial concentrated GT granules. Sensitivity was increased by multi-wavelength detection. The contents of selected marker components in GT granules varied significantly among manufacturers and batches, making it necessary to evaluate the quality of concentrated GT granules in the market.

  5. Analysis of Organic Acids in Blueberry Juice and its Fermented Wine by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hongxue Fu

    2015-08-01

    Full Text Available A rapid analytical method for simultaneous separation and determination of organic acids is of the essence for quality control of blueberry juice and its fermented wine. In this present study, a High Performance Liquid Chromatography (HPLC method for separation and determination of organic acids (oxalic acid, gluconic acid, tartaric acid, formic acid, pyruvic acid, malic acid, isocitric acid, shikimic acid, lactic acid, acetic acid, citric acid, succinic acid and propionic acid in blueberry juice and wine has been developed. The chromatographic separation was performed at 35°C by using an ammonium hydrogen phosphate buffer (pH 2.8 as mobile phase and 0.6 mL/min as the column flow rate. A C18 analytical column and Ultraviolet Detection (UV at &lembda = 210 nm were used for all acids above. The method was validated for linearity, limit of detection, limit of quantification, accuracy and precision. The applicability of the method was demonstrated by analyzing organic acids in real samples of six species of blueberry juices and wines. The results show that species significantly affect distribution of organic acids in samples but not the kinds of organic acids between six species. Oxalic acid, gluconic acid, malic acid, shikimic acid and citric acid are detected in blueberry juice. Citric acid, which accounts for a percentage >75% of the whole content of organic acids, is the major acid in four kinds of tested species (Sharpblue, Misty, Anna and Bluecrop. In the other two species (Britewell and Premier, malic acid, gluconic acid and citric acid own a mean percentage of 40, 32 and 25%, respectively. After yeast fermentation and aging, several new organic acids (pyruvic acid, isocitric acid, lactic acid, acetic acid, succinic acid and propionic acid appear in wine.

  6. Pharmacokinetic study of mangiferin in rat plasma and retina using high-performance liquid chromatography

    Science.gov (United States)

    Hou, Yunlong; Fan, Shengjun; Gu, Yuanqin; Yu, Xuhui; Li, Baoxin

    2010-01-01

    Purpose Although the naturally occurring antioxidant mangiferin has been widely used, it is not yet known whether it can cross the blood-retina barrier (BRB) and enter the eye. The purpose of this experiment was to investigate the ability of mangiferin to pass the blood-retina barrier. Methods Sprague–Dawley rats were used for biologic fluid sampling after intravenous administration of mangiferin at doses of 10, 25, and 50 mg/kg. Blood and retina samples were collected at different time points post-dose. High-performance liquid chromatography (HPLC) separation was conducted on a COSMOSIL 5C18—MS—II column (4.6 mm×250 mm, 5 μm) with a flow rate of 1.0 ml/min using a mobile phase comprised of methanol −2% glacial acetic acid (40:60 v:v). Results The HPLC method has proven suitable to determine the presence of mangiferin in the eye. The plasma concentration of mangiferin was dose dependent. Pharmacokinetic parameters of mangiferin in plasma after intravenous administration were fitted to the two-compartment model with the first-order elimination and first-order transfer between central and peripheral compartments. The concentration of mangiferin in the retina goes with that in the blood. Mangiferin concentrations in the retina reached 5.69±1.48 μg/ml 0.5 h after intravenous administration (50 mg/kg) and then dropped gradually to 0.30±0.02 μg/ml 5.0 h later. The eye–to-plasma concentration ratio was 2.80%. Conclusions Mangiferin can pass the blood-retina barrier after a single intravenous administration and may be a potential natural antioxidant in treating eye diseases. PMID:20806037

  7. Post Column Derivatization Using Reaction Flow High Performance Liquid Chromatography Columns.

    Science.gov (United States)

    Jones, Andrew; Pravadali-Cekic, Sercan; Hua, Stanley; Kocic, Danijela; Camenzuli, Michelle; Dennis, Gary; Shalliker, Andrew

    2016-04-26

    A protocol for the use of reaction flow high performance liquid chromatography columns for methods employing post column derivatization (PCD) is presented. A major difficulty in adapting PCD to modern HPLC systems and columns is the need for large volume reaction coils that enable reagent mixing and then the derivatization reaction to take place. This large post column dead volume leads to band broadening, which results in a loss of observed separation efficiency and indeed detection in sensitivity. In reaction flow post column derivatization (RF-PCD) the derivatization reagent(s) are pumped against the flow of mobile phase into either one or two of the outer ports of the reaction flow column where it is mixed with column effluent inside a frit housed within the column end fitting. This technique allows for more efficient mixing of the column effluent and derivatization reagent(s) meaning that the volume of the reaction loops can be minimized or even eliminated altogether. It has been found that RF-PCD methods perform better than conventional PCD methods in terms of observed separation efficiency and signal to noise ratio. A further advantage of RF-PCD techniques is the ability to monitor effluent coming from the central port in its underivatized state. RF-PCD has currently been trialed on a relatively small range of post column reactions, however, there is currently no reason to suggest that RF-PCD could not be adapted to any existing one or two component (as long as both reagents are added at the same time) post column derivatization reaction.

  8. DNA-based diagnosis of isolated sulfite oxidase deficiency by denaturing high-performance liquid chromatography.

    Science.gov (United States)

    Lam, Ching-Wan; Li, Chi-Keung; Lai, Chi-Kong; Tong, Sui-Fan; Chan, Kwok-Yin; Ng, Grace Sui-Fun; Yuen, Yuet-Ping; Cheng, Anna Wai-Fun; Chan, Yan-Wo

    2002-01-01

    Isolated sulfite oxidase deficiency is a rare autosomal recessive disease, characterized by severe neurological abnormalities, seizures, mental retardation, and dislocation of the ocular lenses, that often leads to death in infancy. There is a special demand for prenatal diagnosis, since no effective treatment is available for isolated sulfite oxidase deficiency. Until now, the cDNA sequence of the sulfite oxidase (SUOX) gene has been available, but the genomic sequence of the SUOX gene has not been published. In this study, we have performed a DNA-based diagnosis of isolated sulfite oxidase deficiency in a Chinese patient. To do so, we designed oligonucleotide primers for amplification of the predicted exons and intron-exon boundaries of the SUOX gene obtained from the completed draft version of the human genome. Using overlapping PCR products, we confirmed the flanking intronic sequences of the coding exons and that the entire 466-residue mature peptide is encoded by the last exon of the gene. We then performed mutation detection using denaturing high-performance liquid chromatography (DHPLC). The DHPLC chromatogram of exon 2b showed the presence of heteroduplex peaks only after mixing of the mutant DNA with the wild-type DNA, indicating the presence of a homozygous mutation. Direct DNA sequencing showed a homozygous base substitution at codon 160, changing the codon from CGG to CAG, which changes the amino acid from arginine to glutamine, i.e., R160Q. The DNA-based diagnosis of isolated sulfite oxidase deficiency will enable us to make an accurate determination of carrier status and to perform prenatal diagnosis of this disease. The availability of the genomic sequences of human genes from the completed draft human genome sequence will simplify the development of molecular genetic diagnoses of human diseases from peripheral blood DNA.

  9. Analysis of Some Pesticide Residues in Cauliflower by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Sheheli Islam

    2009-01-01

    Full Text Available Problem statement: Increased use of chemicals on vegetables started gaining momentum and continued its up-trend in Bangladesh. Wide spread use of pesticides in agriculture concern of residue accumulation, which may remain in food and agricultural environment causing concern of human health and risking ecological balance. Attempt made to ensure that their applications were correct and safe and result in no residues in food beyond codex developed maximum residue limits. Approach: This study reported a method based on High Performance Liquid Chromatography (HPLC for determination of pesticide residues used in Cauliflower. Cauliflower sprayed with, 4 different pesticides (diazinon, malathion, chlorpyrifos and cypermethrin at recommended dose and double of recommended dose were analyzed for their residual contents. Samples were collected at same day after application of pesticide. Commercial samples of cauliflowers were collected from different markets of Dhaka city. Reversed-phase HPLC system with UV detection was used for the separation, identification and quantification of all these analytes using acetonitrile-water (70:30, v/v as mobile phase. Results: Limit of detection of 0.02 mg kg-1 was obtained. Calibration curves that constructed for the analytes spiked into samples followed linear relationships with good correlation coefficients (R2>0.990. In the analysis, from vegetables treated with diazinon and chlorpyrifos at recommended and double of recommended doses, residual amounts above respective MRL values were found. Conclusion: Method used permitted the determination of these pesticides in cauliflower at concentration level demanded by current legislation. Attention paid on excess use or abuse of pesticides by judicious application for safety of public health in Bangladesh. Additional data to monitor residues in food and to fill gaps in current knowledge would be helpful in assessing human exposure risks from ingestion of contaminated

  10. Dynamic Behavior of Clobazam on High-Performance Liquid Chromatography Chiral Stationary Phases.

    Science.gov (United States)

    Sabia, Rocchina; De Martino, Michela; Cavazzini, Alberto; Villani, Claudio

    2016-01-01

    Clobazam, a 1,5-benzodiazepin-2,4-dione, is a chiral molecule because its ground state conformation features a nonplanar seven-membered ring lacking reflection symmetry elements. The two conformational enantiomers of clobazam interconvert at room temperature by a simple ring-flipping process. Variable temperature HPLC on the Pirkle type (R)-N-(3,5-dinitronenzoyl)phenylglycine and (R,R)-Whelk-O1 chiral stationary phases (CSPs) allowed us to separate for the first time the conformational enantiomers of clobazam and to observe peak coalescence-decoalescence phenomena due to concomitant separation and interconversion processes occurring on the same time scale. Clobazam showed temperature dependent dynamic high-performance liquid chromatography (HPLC) profiles with interconversion plateaus on the two CSPs indicative of on-column enantiomer interconversion. (enantiomerization) in the column temperature range between Tcol = 10°C and Tcol = 30°C, whereas on-column interconversion was absent at temperature close to or lower than Tcol = 5°C. Computer simulation of exchange-deformed HPLC profiles using a program based on the stochastic model yielded the apparent rate constants for the on-column enantiomerization and the corresponding free energy activation barriers. At Tcol = 20°C the averaged enantiomerization barriers, ΔG(‡), for clobazam were found in the range 21.08-21.53 kcal mol(-1) on the two CSPs. The experimental dynamic chromatograms and the corresponding interconversion barriers reported in this article are consistent with the literature data measured by DNMR at higher temperatures and in different solvents.

  11. Dispersive liquid-liquid microextraction based on solidification of floating organic droplets followed by high performance liquid chromatography for the determination of duloxetine in human plasma.

    Science.gov (United States)

    Suh, Joon Hyuk; Lee, Yun Young; Lee, Hee Joo; Kang, Myunghee; Hur, Yeoun; Lee, Sun Neo; Yang, Dong-Hyug; Han, Sang Beom

    2013-03-05

    A novel dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) technique was developed for the determination of duloxetine in human plasma samples by high performance liquid chromatography with fluorescence detection (HPLC-FLD). During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. After the protein precipitation step, duloxetine in an alkaline sample solution was quickly extracted by DLLME-SFO with 50 μL of 1-undecanol (extractant). Disperser was unnecessary because the small amount of remaining acetonitrile, which acts as a protein precipitating reagent, was also employed as a disperser; therefore, organic solvent consumption was reduced as much as possible. The emulsion was centrifuged and then fine droplets were floated to the top of the sample solution. The floated droplets were solidified in an ice bath and easily transferred. Various DLLME-SFO parameters such as extractant type, extractant amount, ionic strength, pH and extraction time were optimized. The chromatographic separation of duloxetine was carried out using ethanol as mobile phase. Validation of the method was performed with respect to linearity, intra- and inter-day accuracy and precision, limit of quantification (LOQ), and recovery. Calibration curves for duloxetine showed good linearity with correlation coefficients (r²) higher than 0.99. The method showed good precision and accuracy, with intra- and inter-assay coefficients of variation less than 15% (LOQ: less than 20%) at all concentrations. The recovery was carried out following the standard addition procedure with yields ranging from 59.6 to 65.5%. A newly developed environmentally friendly method was successfully applied to the pharmacokinetic study of duloxetine in human plasma and was shown to be an alternative green approach compared with the conventional solid-phase microextraction (SPME) and dispersive

  12. 高压液相色谱法测定纸质食品接触材料中亚甲基双硫氰酸酯的迁移量%Determination of methylene dithiocyanate migration from food contact paper materials by high pressure liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    丁岚; 马强; 李文涛; 马会娟; 李晶瑞; 孟宪双; 陈云霞; 白桦

    2013-01-01

      目的建立纸质食品接触材料中亚甲基双硫氰酸酯迁移量的高压液相色谱测定方法。方法食品模拟物(水、3%乙酸水溶液、10%乙醇水溶液和橄榄油)中的亚甲基双硫氰酸酯通过高压液相色谱进行分离,采用二极管阵列检测器进行测定。水基食品模拟物直接进样,油基食品模拟物经乙腈萃取后进样,外标法定量。结果3种水基食品模拟物中,亚甲基双硫氰酸酯在0.5~50 mg/L范围内线性关系良好,定量下限为0.5 mg/L,平均回收率为88.2%~97.4%,相对标准偏差为0.44%~6.54%;油基食品模拟物中,亚甲基双硫氰酸酯在1.0~20 mg/kg范围内线性关系良好,定量下限为1.0 mg/kg,平均回收率为99.3%~104.7%,相对标准偏差为0.75%~3.15%。结论该方法准确、简便、快速,可用于纸质食品接触材料中亚甲基双硫氰酸酯迁移量的实际检验工作。%Objective An analytical method for the detection of methylene dithiocyanate migration from food contact paper materials by high pressure liquid chromatography was established. Methods Methylene dithiocyanate migrated into the food simulants (water, 3%aqueous acetic acid solution, 10%aqueous ethanol solution and refined olive oil) was separated and detected by high pressure liquid chromatography coupled with diode array detector. The water-based food simulants were subjected to instrumental analysis directly and the oil-based food simulant was extracted by acetonitrile and then analyzed and quantitated with external standard method. Results This method showed a good linearity for methylene dithiocyanate in the range of 0.5~50 mg/L in the 3 water-based food simulants with the limit of quantification of 0.5 mg/L. The mean recoveries at three spiked levels were in the range of 88.2%~97.4%with relative standard deviations of 0.44%~6.54%. Me-thylene dithiocyanate exhibited a good linearity in the range of 1.0~20 mg/kg with the limit of quantification of 1.0 mg/kg. The mean

  13. Determination of caffeoylquinic acids in feed and related products by focused ultrasound solid-liquid extraction and ultra-high performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Tena, M T; Martínez-Moral, M P; Cardozo, P W

    2015-06-26

    A method to determine caffeoylquinic acids (CQAs) in three sources (herbal extract, feed additive and finished feed) using for the first time focused ultrasound solid-liquid extraction (FUSLE) followed by ultra-high performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry is presented. Pressurized liquid extraction (PLE) was also tested as extraction technique but it was discarded because cynarin was not stable under temperature values used in PLE. The separation of the CQAs isomers was carried out in only seven minutes. FUSLE variables such as extraction solvent, power and time were optimized by a central composite design. Under optimal conditions, FUSLE extraction was performed with 8mL of an 83:17 methanol-water mixture for 30s at a power of 60%. Only two extraction steps were found necessary to recover analytes quantitatively. Sensitivity, linearity, accuracy and precision were established. Matrix effect was studied for each type of sample. It was not detected for mono-CQAs, whereas the cynarin signal was strongly decreased due to ionization suppression in presence of matrix components; so the quantification by standard addition was mandatory for the determination of di-caffeoylquinic acids. Finally, the method was applied to the analysis of herbal extracts, feed additives and finished feed. In all samples, chlorogenic acid was the predominant CQA, followed by criptochlorogenic acid, neochlorogenic acid and cynarin. The method allows an efficient determination of chlorogenic acid with good recovery rates. Therefore, it may be used for screening of raw material and for process and quality control in feed manufacture.

  14. Pipette vial dispersive liquid-liquid microextraction combined with high-performance liquid chromatography for the determination of benzoylurea insecticide in fruit juice.

    Science.gov (United States)

    Xi, Xuefei; Yang, Miyi; Shen, Ganni; Wu, Xiaoling; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

    2016-01-01

    A simple, sensitive, and efficient method of using a pipette vial to perform dispersive liquid-liquid microextraction based on the solidification of floating organic droplets was coupled with high-performance liquid chromatography (HPLC) and a diode array detector for the preconcentration and analysis of four benzoylurea insecticides in fruit juice. In this method, 1-dodecanol was used as an extractant, and a snipped pipette was used as an experimental vial to simplify the procedure of collecting and separating solidified extractant. The experimental parameters were optimized using a Plackett-Burman design and one-factor-at-a-time method. Under the optimal conditions in the water model, the limits of detection for analytes varied from 0.03 to 0.28 μg/L, and the enrichment factors ranged from 147 to 206. Linearity was achieved for diflubenzuron and flufenoxuron in a range of 0.5-500 μg/L, for hexaflumuron in a range of 1-500 μg/L, and for triflumuron in a range of 5-500 μg/L. The correlation coefficients for the analytes ranged from 0.9986 to 0.9994 with recoveries of 91.4-110.9%. Finally, the developed technique was successfully applied to fruit juice samples with acceptable results. The relative standard deviations of the analytes at two spiking levels (50 and 200 μg/L) varied between 0.2 and 4.5%.

  15. Sensitive determination of melamine in milk and powdered infant formula samples by high-performance liquid chromatography using dabsyl chloride derivatization followed by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Faraji, M; Adeli, M

    2017-04-15

    A new and sensitive pre-column derivatization with dabsyl chloride followed by dispersive liquid-liquid microextraction was developed for the analysis of melamine (MEL) in raw milk and powdered infant formula samples by high performance liquid chromatography (HPLC) with visible detection. Derivatization with dabsyl chloride leads to improving sensitivity and hydrophobicity of MEL. Under optimum conditions of derivatization and microextraction steps, the method yielded a linear calibration curve ranging from 1.0 to 500μgL(-1) with a determination coefficient (R(2)) of 0.9995. Limit of detection and limit of quantification were 0.1 and 0.3μgL(-1), respectively. The relative standard deviation (RSD%) for intra-day (repeatability) and inter-day (reproducibility) at 25 and 100μgL(-1) levels of MEL was less than 7.0% (n=6). Finally, the proposed method was successfully applied for the preconcentration and determination of MEL in different raw milk and powdered infant formula, and satisfactory results were obtained (relative recovery ⩾94%).

  16. Ion pair-based dispersive liquid-liquid microextraction followed by high performance liquid chromatography as a new method for determining five folate derivatives in foodstuffs.

    Science.gov (United States)

    Nojavan, Yones; Kamankesh, Marzieh; Shahraz, Farzaneh; Hashemi, Maryam; Mohammadi, Abdorreza

    2015-05-01

    A novel technique for simultaneous determination of five folate derivatives in various food matrices was developed by ion pair-based dispersive liquid-liquid microextraction (IP-DLLME) combined with high-performance liquid chromatography (HPLC). In the proposed method, N-methyl-N,N-dioctyloctan-1-ammonium chloride (aliquat-336) was used as an ion-pair reagent. Effective variables of microextraction process were optimized. Under optimum conditions, the method yielded a linear calibration curve ranging from 1-200 ng g(-1) with correlation coefficients (r(2)) higher than 0.98. The relative standard deviation for the seven analyses was 5.2-7.4%. Enrichment factors for the five folates ranged between 108-135. Limits of detection were 2-4.1 ng g(-1). A comparison of this method with other methods described that the new proposed method is rapid and accurate, and gives very good enrichment factors and detection limits for determining five folate derivatives. The newly developed method was successfully applied for the determination of five folate derivatives in wheat flour, egg yolk and orange juice samples.

  17. Intravascular Residence Time Determination for the Cyanide Antidote Dimethyl Trisulfide in Rat by Using Liquid-Liquid Extraction Coupled with High Performance Liquid Chromatography

    Science.gov (United States)

    De Silva, Deepthika; Lee, Steven; Duke, Anna; Angalakurthi, Siva; Chou, Ching-En; Ebrahimpour, Afshin; Thompson, David E.

    2016-01-01

    These studies represent the first report on the intravascular residence time determinations for the cyanide antidote dimethyl trisulfide (DMTS) in a rat model by using high performance liquid chromatography coupled with ultraviolet absorption spectroscopy (HPLC-UV). The newly developed sample preparation included liquid-liquid extraction by cyclohexanone. The calibration curves showed a linear response for DMTS concentrations between 0.010 and 0.30 mg/mL with R2 = 0.9994. The limit of detection for DMTS via this extraction method was 0.010 mg/mL, and the limit of quantitation was 0.034 mg/mL. Thus this calibration curve provided a tool for determining DMTS in the range between 0.04 and 0.30 mg/mL. Rats were given 20 mg/kg DMTS dose (in 15% Polysorbate 80) intravenously, and blood samples were taken 15, 60, 90, 120, and 240 min after DMTS injections. The data points were plotted as DMTS concentration in RBCs versus time, and the intravascular residence time was determined graphically. The results indicated a half-life of 36 min in a rat model, suggesting that the circulation time is long enough to provide a reasonable time interval for cyanide antagonism. PMID:28053802

  18. Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Jia, Xiaoyu; Han, Yi; Liu, Xinli; Duan, Taicheng; Chen, Hangting

    2011-01-01

    The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg +) and mercury (Hg 2+) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg + and Hg 2+ were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL -1 for MeHg + and 0.0014 ng mL -1 for Hg 2+, respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL -1 MeHg + and Hg 2+ were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

  19. Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

    Science.gov (United States)

    Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

    2017-04-14

    An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg(+)), ethylmercury (EtHg(+)) and inorganic mercury (Hg(2+)) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL(-1) for EtHg(+) and 5-450ngL(-1) for MeHg(+) and Hg(2+). Limits of detection were 3.0ngL(-1) for EtHg(+) and 1.5ngL(-1) for MeHg(+) and Hg(2+). Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%.

  20. Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jia Xiaoyu; Han Yi; Liu Xinli [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Graduate School of Chinese Academy of Sciences, Beijing 100039 (China); Duan Taicheng, E-mail: tcduan@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Chen Hangting, E-mail: htchen@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China)

    2011-01-15

    The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg{sup +}) and mercury (Hg{sup 2+}) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg{sup +} and Hg{sup 2+} were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL{sup -1} for MeHg{sup +} and 0.0014 ng mL{sup -1} for Hg{sup 2+}, respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL{sup -1} MeHg{sup +} and Hg{sup 2+} were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

  1. Simultaneous determination of six synthetic phenolic antioxidants in edible oils using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography with diode array detection.

    Science.gov (United States)

    Xu, Shuangjiao; Liu, Liangliang; Wang, Yanqin; Zhou, Dayun; Kuang, Meng; Fang, Dan; Yang, Weihua; Wei, Shoujun; Xiao, Aiping; Ma, Lei

    2016-08-01

    A simple, rapid, organic-solvent- and sample-saving pretreatment technique, called dispersive liquid-liquid microextraction, was developed for the determination of six synthetic phenolic antioxidants from edible oils before high-performance liquid chromatography with diode array detection. The entire procedure was composed of a two-step microextraction and a centrifugal process and could be finished in about 5 min, only consuming only 25 mg of sample and 1 mL of the organic solvent for each extraction. The influences of several important parameters on the microextraction efficiency were thoroughly investigated. Recovery assays for oil samples were spiked at three concentration levels, 50, 100 and 200 mg/kg, and provided recoveries in the 86.3-102.5% range with a relative standard deviation below 3.5%. The intra-day and inter-day precisions for the analysis were less than 3.8%. The proposed method was successfully applied for the determination of synthetic phenolic antioxidants in different oil samples, and satisfactory results were obtained. Thus, the developed method represents a viable alternative for the quality control of synthetic phenolic antioxidant concentrations in edible oils.

  2. Intravascular Residence Time Determination for the Cyanide Antidote Dimethyl Trisulfide in Rat by Using Liquid-Liquid Extraction Coupled with High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Deepthika De Silva

    2016-01-01

    Full Text Available These studies represent the first report on the intravascular residence time determinations for the cyanide antidote dimethyl trisulfide (DMTS in a rat model by using high performance liquid chromatography coupled with ultraviolet absorption spectroscopy (HPLC-UV. The newly developed sample preparation included liquid-liquid extraction by cyclohexanone. The calibration curves showed a linear response for DMTS concentrations between 0.010 and 0.30 mg/mL with R2 = 0.9994. The limit of detection for DMTS via this extraction method was 0.010 mg/mL, and the limit of quantitation was 0.034 mg/mL. Thus this calibration curve provided a tool for determining DMTS in the range between 0.04 and 0.30 mg/mL. Rats were given 20 mg/kg DMTS dose (in 15% Polysorbate 80 intravenously, and blood samples were taken 15, 60, 90, 120, and 240 min after DMTS injections. The data points were plotted as DMTS concentration in RBCs versus time, and the intravascular residence time was determined graphically. The results indicated a half-life of 36 min in a rat model, suggesting that the circulation time is long enough to provide a reasonable time interval for cyanide antagonism.

  3. Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

    2013-07-26

    A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals.

  4. Rapid extraction and determination of amphetamines in human urine samples using dispersive liquid-liquid microextraction and solidification of floating organic drop followed by high performance liquid chromatography.

    Science.gov (United States)

    Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba

    2014-06-01

    A novel, rapid, simple and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine amphetamine and methamphetamine in urine samples. The factors affecting the extraction efficiency of DLLME-SFO such as the kind and volume of the extraction and the disperser solvents, effect of concentration of K2CO3 and extraction time were investigated and the optimal extraction conditions were established. Under the optimum conditions (extraction solvent: 30.0μl 1-undecanol; disperser solvent: 300μl acetonitrile; buffer concentration: 2% (w/v) K2CO3 and extraction time: 1min), calibration curves are linear in the range of 10-3000μgl(-1) and limit of detections (LODs) are in the range of 2-8μgl(-1). The relative standard deviations (RSDs) for 100μgl(-1) of amphetamine and methamphetamine in diluted urine are in the range of 6.2-7.8% (n=7). The method was successfully applied for the determination of amphetamine and methamphetamine in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 87.8-113.2%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of amphetamine and methamphetamine in urine.

  5. Novel method for the determination of five carbamate pesticides in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    Zhi Mei Liu; Xiao Huan Zang; Wei Hua Liu; Chun Wang; Zhi Wang

    2009-01-01

    A novel method for the determination of five carbamate pesticides(metolcarb,carbofuran,carbaryl,isoprocard and diethofencard)in water samples was developed by dispersive liquid-liquid microextraction(DLLME)coupled with high performance liquid chromatography-diode array detector(HPLC-DAD).Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results.Under the optimum conditions for the method,the calibration curve was linear in the concentration range from 5 to I000 ng mL-1 for all the five carbamate pesticides,with the correlation coefficients(r2)varying from 0.9984 to 0.9994.Good enrichment factors were achieved ranging from 80 to 177-fold,depending on the compound.The limits of detection(LODs)(S/N = 3)were ranged from 0.1 to 0.5 ng mL-1.The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.

  6. Rapid resolution liquid chromatography-mass spectrometry and high-performance liquid chromatography-fluorescence detection for metabolism and pharmacokinetic studies of ergosta-4,6,8(14),22-tetraen-3-one.

    Science.gov (United States)

    Zhao, Ying-Yong; Qin, Xiang-Yang; Cheng, Xian-Long; Liu, Xue-Ying; Lin, Rui-Chao; Zhang, Yongmin; Li, Xiao-Ye; Sun, Xiao-Li; Sun, Wen-Ji

    2010-08-24

    Ergosta-4,6,8(14),22-tetraen-3-one (ergone) from many medicinal plants has been demonstrated to possess a variety of pharmacological activities in vivo and in vitro, including cytotoxic, diuretic and immunosuppressive activity. Metabolism and pharmacokinetic studies on rat were conducted for ergone. Rapid resolution liquid chromatography with atmospheric pressure chemical ionization tandem multi-stage mass spectrometry (RRLC-APCI-MS(n)) and high-performance liquid chromatography with fluorescence detection (HPLC-FLD) methods were applied for the identification and quantification of ergone and its metabolite from rat plasma, faeces and urine. A metabolite was identified by RRLC-DAD-APCI-MS(n): 22,23-epoxy-ergosta-4,6,8(14)-triaen-3-one (epoxyergone). The concentrations of the analyte with its metabolites were determined by HPLC-FLD at excitation wavelength of 370 nm and emission wavelength of 485 nm. The samples were deproteinized with methanol after addition of camptothecin as internal standard (IS). The analysis was performed on a Diamonsil C18 column (150 mm x 4.6 mm x 5 microm) with a mobile phase gradient consisting of methanol and water at a flow rate of 1 mL min(-1). The assay was linear over the concentration range of 42-1500, 36-7500 and 42-1500 ng mL(-1) for plasma, faecal homogenate and urine respectively. The absolute recoveries were found to be 97.0+/-1.2%, 98.1+/-0.7% and 96.6+/-1.8% for plasma, faecal homogenate and urine respectively. The intra-day and inter-day relative standard deviations (RSD) were less than 10%. The previous HPLC-MS/MS method is not affordable for most laboratories because of the specialty requirement and high equipment cost. However, the HPLC-FLD method is economic and operating simply for quantitative determination of ergone and its metabolite in rat plasma, faeces and urine. In addition, liquid chromatography coupled with ion trap multi-stage mass spectrometry is becoming a useful technique for ergone metabolite identification.

  7. Recent Experimental Efforts on High-Pressure Supercritical Injection for Liquid Rockets and Their Implications

    Directory of Open Access Journals (Sweden)

    Bruce Chehroudi

    2012-01-01

    Full Text Available Pressure and temperature of the liquid rocket thrust chambers into which propellants are injected have been in an ascending trajectory to gain higher specific impulse. It is quite possible then that the thermodynamic condition into which liquid propellants are injected reaches or surpasses the critical point of one or more of the injected fluids. For example, in cryogenic hydrogen/oxygen liquid rocket engines, such as Space Shuttle Main Engine (SSME or Vulcain (Ariane 5, the injected liquid oxygen finds itself in a supercritical condition. Very little detailed information was available on the behavior of liquid jets under such a harsh environment nearly two decades ago. The author had the opportunity to be intimately involved in the evolutionary understanding of injection processes at the Air Force Research Laboratory (AFRL, spanning sub- to supercritical conditions during this period. The information included here attempts to present a coherent summary of experimental achievements pertinent to liquid rockets, focusing only on the injection of nonreacting cryogenic liquids into a high-pressure environment surpassing the critical point of at least one of the propellants. Moreover, some implications of the results acquired under such an environment are offered in the context of the liquid rocket combustion instability problem.

  8. Determination of Vanillin from Tincture and Extract Products of Vanilla by Using Reversed Phase High Pressure Liquid Chromatography%反相高效液相色谱法检测香草兰豆酊、浸膏中香兰素

    Institute of Scientific and Technical Information of China (English)

    卢少芳; 初众; 赵建平

    2009-01-01

    采用反相高效液相色谱法测定香草兰豆酊、浸膏中香兰素含量,色谱柱为C_(18)柱,甲醇/0.5%冰乙酸水溶液(20/80.v/v)为流动相,等浓度洗脱,测定波长为280 nm,外标法定量.该方法相对标准偏差分别为0.28%和0.24%.加标回收率为97.89%~100.71%.本方法具有操作简便,结果准确等优点,特别适用于香草兰豆酊、浸膏等精深加工产品中香兰素含量的检测分析.%A simple, rapid and accurate method was developed for determination of vanillin by Reversed Phase High Pressure Liquid Chromatography. In this method chromatographic column was C18, mobile phase methanol/0.5% acetic acid (20/80, v/v), elution isocratic, wavelength 280nm, External Standard for quantification. With this method the relative standard deviation was 0.28% for detection of the samples of vanilla tincture and 0.24% for detection of the samples of vanilla extract, and the spike recovery rate ranged from 98.89% to 100.71%. This method is good for determination of vanillin from the well-processed vanilla tincture and the vanilla extract.

  9. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 1: method of analysis.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition.

  10. [Determination of congo red in beef by high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry].

    Science.gov (United States)

    Lin, Hui; Xu, Chunxiang; Yan, Chunrong; Zhang, Zheng; Wang, Suilou

    2013-09-01

    A method was developed for the determination of congo red in beef. The analyte was identified by high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry (LC-QTOF MS) and quantitatively determined by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the congo red in the beef sample was separated on an Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HD UPLC column (50 mm x 2.1 mm, 1.8 microm) HPLC , using 95% (volume percentage) methanol as the mobile phase at 0.2 mL/min. The detection was performed on an AB 4000 + triple quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM) mode. The results showed that the linear range of congo red mass concentration was 0.03 - 1 mg/L with the correlation coefficient of 0.999 8. The method had a good precision with the RSDs lower than 5% and the recoveries ranging from 88% to 91%. The limit of detection (LOD) of congo red was 0.01 mg/L. With good reproducibility, the method is simple, fast and effective for the determination of the illegally added congo red in beef and other meat products.

  11. Gas-Liquid Mass Transfer in a Slurry Bubble Column Reactor under High Temperature andHigh Pressure

    Institute of Scientific and Technical Information of China (English)

    杨卫国; 王金福; 金涌

    2001-01-01

    The gas-liquid mass transfer of H2 and CO in a high temperature and high-pressure three-phase slurry bubble column reactor is studied. The gas-liquid volumetric mass transfer coefficients kLa are obtained by measuring the dissolution rate of H2 and CO. The influences of the main operation conditions, such as temperature, pressure,superficial gas velocity and solid concentration, are studied systematically. Two empirical correlations are proposed to predict kLa values for H2 and CO in liquid paraffln/solid particles slurry bubble column reactors.

  12. High Performance Liquid Chromatography-mass Spectrometry Analysis of High Antioxidant Australian Fruits with Antiproliferative Activity Against Cancer Cells

    Science.gov (United States)

    Sirdaarta, Joseph; Maen, Anton; Rayan, Paran; Matthews, Ben; Cock, Ian Edwin

    2016-01-01

    g/mL). All other extracts were nontoxic. A total of 145 unique mass signals were detected in the lemon aspen methanolic and aqueous extracts by nonbiased high-performance liquid chromatography-mass spectrometry analysis. Of these, 20 compounds were identified as being of particular interest due to their reported antioxidant and/or anticancer activities. Conclusions: The lack of toxicity and antiproliferative activity of the high antioxidant plant extracts against HeLa and CaCo2 cancer cell lines indicates their potential in the treatment and prevention of some cancers. SUMMARY Australian fruit extracts with high antioxidant contents were potent inhibitors of CaCo2 and HeLa carcinoma cell proliferationMethanolic lemon aspen extract was particularly potent, with IC50 values of 480 μg/mL (HeLa) and 769 μg/mL (CaCo2)High-performance liquid chromatography-mass spectrometry-quadrupole time-of-flight analysis highlighted and putatively identified 20 compounds in the antiproliferative lemon aspen extractsIn contrast, lower antioxidant content extracts stimulated carcinoma cell proliferationAll extracts with antiproliferative activity were nontoxic in the Artemia nauplii assay. Abbreviations used: DPPH: di (phenyl)- (2,4,6-trinitrophenyl) iminoazanium, HPLC: High-performance liquid chromatography, IC50: The concentration required to inhibit by 50%, LC50: The concentration required to achieve 50% mortality, MS: Mass spectrometry. PMID:27279705

  13. Trace analysis of selected hormones and sterols in river sediments by liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.

    Science.gov (United States)

    Matić, Ivana; Grujić, Svetlana; Jauković, Zorica; Laušević, Mila

    2014-10-17

    In this paper, development and optimization of new LC-MS method for determination of twenty selected hormones, human/animal and plant sterols in river sediments were described. Sediment samples were prepared using ultrasonic extraction and clean up with silica gel/anhydrous sodium sulphate cartridge. Extracts were analyzed by liquid chromatography-linear ion trap-tandem mass spectrometry, with atmospheric pressure chemical ionization. The optimized extraction parameters were extraction solvent (methanol), weight of the sediment (2 g) and time of ultrasonic extraction (3× 10 min). Successful chromatographic separation of hormones (estriol and estrone, 17α- and 17β-estradiol) and four human/animal sterols (epicoprostanol, coprostanol, α-cholestanol and β-cholestanol) that have identical fragmentation reactions was achieved. The developed and optimized method provided high recoveries (73-118%), low limits of detection (0.8-18 ng g(-1)) and quantification (2.5-60 ng g(-1)) with the RSDs generally lower than 20%. Applicability of the developed method was confirmed by analysis of six river sediment samples. A widespread occurrence of human/animal and plant sterols was found. The only detected hormone was mestranol in just one sediment sample.

  14. Determination of organophosphorus flame retardants in fish by pressurized liquid extraction using aqueous solutions and solid-phase microextraction coupled with gas chromatography-flame photometric detector.

    Science.gov (United States)

    Gao, Zhanqi; Deng, Yuehua; Yuan, Wenting; He, Huan; Yang, Shaogui; Sun, Cheng

    2014-10-31

    A novel method was developed for the determination of organophosphorus flame retardants (PFRs) in fish. The method consists of a combination of pressurized liquid extraction (PLE) using aqueous solutions and solid-phase microextraction (SPME), followed by gas chromatography-flame photometric detector (GC-FPD). The experimental parameters that influenced extraction efficiency were systematically evaluated. The optimal responses were observed by extracting 1g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150°C for 5min and acid-washed silica gel used as lipid sorbent. The obtained extract was then analyzed by SPME coupled with GC-FPD without any additional clean-up steps. Under the optimal conditions, the proposed procedure showed a wide linear range (0.90-5000ngg(-1)) obtained by analyzing the spiked fish samples with increasing concentrations of PFRs and correlation coefficient (R) ranged from 0.9900 to 0.9992. The detection limits (S/N=3) were in the range of 0.010-0.208ngg(-1) with standard deviations (RSDs) ranging from 2.0% to 9.0%. The intra-day and inter-day variations were less than 9.0% and 7.8%, respectively. The proposed method was successfully applied to the determination of PFRs in real fish samples with recoveries varying from 79.8% to 107.3%. The results demonstrate that the proposed method is highly effective for analyzing PFRs in fish samples.

  15. Analysis of alkylresorcinols in cereal grains and products using ultrahigh-pressure liquid chromatography with fluorescence, ultraviolet, and CoulArray electrochemical detection.

    Science.gov (United States)

    Ross, Alastair B

    2012-09-12

    Alkylresorcinols are phenolic lipids, with homologues ranging from C17 to C25, found in high concentrations in whole grain wheat and rye, lower concentrations in barley, and negligible concentrations in refined wheat flour. The analysis of alkylresorcinols is of importance due to their potential as biomarkers of whole grain intake and emerging evidence for some biological effects. Present HPLC methods have insufficient resolution for accurately quantitating the mix of alkyl- and alkenylresorcinols found in rye. An ultrahigh-pressure liquid chromatography method was developed, and three detection methods (CoulArray (CAED), ultraviolet (UV), and fluorescence detection (FD)) were compared for cereal alkylresorcinol analysis. The lower limits of quantitation and detection were 50 and 20 pg injected, 5 pg and 2 pg injected, and 500 and 1250 pg injected for FD, CAED, and UV, respectively. FD and CAED provided similar results, with some bias for higher results with FD (<10% difference). UV detection generally resulted in overestimation of alkylresorcinol concentrations. The method was applied to cereal (15) and cereal product (90) samples mainly from the United States with results in the same range as previous methods. The improved resolution with this method allows facile analysis of alkylresorcinols from cereal products, including minor unsaturated homologues such as those found in rye.

  16. Factors influencing the separation of oligonucleotides using reversed-phase/ion-exchange mixed-mode high performance liquid chromatography columns.

    Science.gov (United States)

    Biba, Mirlinda; Jiang, Eileen; Mao, Bing; Zewge, Daniel; Foley, Joe P; Welch, Christopher J

    2013-08-23

    New mixed-mode columns consisting of reversed-phase and ion-exchange separation modes were evaluated for the analysis of short RNA oligonucleotides (∼20mers). Conventional analysis for these samples typically involves using two complementary methods: strong anion-exchange liquid chromatography (SAX-LC) for separation based on charge, and ion-pair reversed-phase liquid chromatography (IP-RPLC) for separation based on hydrophobicity. Recently introduced mixed-mode high performance liquid chromatography (HPLC) columns combine both reversed-phase and ion-exchange modes, potentially offering a simpler analysis by combining the benefits of both separation modes into a single method. Analysis of a variety of RNA oligonucleotide samples using three different mixed-mode stationary phases showed some distinct benefits for oligonucleotide separation and analysis. When using these mixed-mode columns with typical IP-RPLC mobile phase conditions, such as ammonium acetate or triethylammonium acetate as the primary ion-pair reagent, the separation was mainly based on the IP-RPLC mode. However, when changing the mobile phase conditions to those more typical for SAX-LC, such as salt gradients with NaCl or NaBr, very different separation patterns were observed due to mixed-mode interactions. In addition, the Scherzo SW-C18 and SM-C18 columns with sodium chloride or sodium bromide salt gradients also showed significant improvements in peak shape.

  17. Molecular Dynamics Simulations of Liquid Phosphorus at High Temperature and Pressure

    Institute of Scientific and Technical Information of China (English)

    WU Yan-Ning; ZHAO Gang; LIU Chang-Song; ZHU Zhen-Gang

    2008-01-01

    By performing ab initio molecular dynamics simulations, we have investigated the mierostructure, dynam-ical and electronic properties of liquid phosphorus (P) under high temperature and pressure. In our simulations, the calculated coordination number (CN) changes discontinuously with density, and seems to increase rapidly after liquid P is compressed to 2.5 g/cm3. Under compression, liquid P shows the first-order liquid-liquid phase transition from the molecular liquid composed of the tetrahedral P4 molecules to complex polymeric form with three-dimensional network structure, accompanied by the nonmetal to metal transition of the electronic structure. The order parameters Q6 and Q4 are sensitive to the microstructural change of liquid P. By calculating diffusion coefficients, we show the dynamical anomaly of liquid P by compression. At lower temperatures, a maximum exists at the diffusion coefficients as a function of density; a