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Sample records for acid determination metodos

  1. Determination of the biodiesel acidity index by potentiometric titration by using different methods; Determinacao do indice de acidez de biodiesel por titulacao potenciometrica utilizando-se diferentes metodos

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    Goncalves, Mary Ane; Sobral, Sidney Pereira; Borges, Paulo Paschoal [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (DIMCI/INMETRO), Duque de Caxias, RJ (Brazil). Diretoria de Metrologia Cientifica e Industrial], E-mail: magoncalves@inmetro.gov.br

    2009-07-01

    This work determined the index of the soybean/fat bio diesel through the potentiometric titration. Four different methods were used with variation of solvent and electrodes. The results were compared by F and t (Student) and it was verified that they were agreed in a 95% confidence interval.

  2. An analytical method for determination of mercury by cold vapor atomic absorption spectroscopy; Determinazione di mercurio. Metodo per spettrometria di assorbimento atomico a vapori freddi (CV-AAS)

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    Campanella, L. [Rome Univ. La Sapienza, Rome (Italy); Mastroianni, D.; Capri, S.; Pettine, M. [CNR, Rome (Italy). Ist. di Ricerca sulle Acque; Spezia, S.; Bettinelli, M. [ENEL, Unified Modelling Language, Piacenza (Italy)

    1999-09-01

    An analytical procedure for the determination of total mercury in wastewaters and natural waters is described. Aqueous samples are fast digested with nitric acid by using the microwave-oven technique; the analysis of mercury is then performed by cold vapor atomic absorption spectrometry (CV-AAS) using two possible instrumental apparatus (batch system or flow injection). Sodium borohydride is used as the reducing agent for mercury in solution (Method A). The use of amalgamation traps on gold for the preconcentration of mercury lowers the detection limit of the analyte (Method B). [Italian] Viene descritta una procedura analitica per la determinazione del mercurio totale in acque di scarico e naturali. Il campione acquoso viene sottoposto a mineralizzazione con acido nitrico in forno a microonde e analizzato mediante spettroscopia di assorbimento atomico a vapori freddi (CV-AAS) in due possibili configurazioni strumentali (sistema batch oppure flow injection), utilizzando sodio boro idruro come agente riducente del mercurio (metodo A). L'impiego della trappola di oro per la preconcentrazione del mercurio mediante amalgama consente di determinare l'analita a livelli di pochi ng/L (metodo B).

  3. Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase); Optimizacion del Metodo Analitico mediante HPLC/UV Operando en Fase Inversa para la Determinacion de Acido Galico y Acido Picrico en Muestras de Origen Pirotecnico

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    Garcia Alonso, S.; Perez Pastor, R. M.

    2013-10-01

    A study on the optimization and development of a chromatographic method for the determination of gallic and picric acids in pyrotechnic samples is presented. In order to achieve this, both analytical conditions by HPLC with diode detection and extraction step of a selected sample were studied. (Author)

  4. Development of an analytic method for arsenic's determination in lime and tortilla; Desarrollo de un metodo analitico para determinacion de arsenico en cal y tortilla

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    Huato Soberanis, Julio; Ogura, Tetsuya [Universidad Autonoma de Guadalajara, Guadalajara, Jalisco (Mexico)

    1995-02-01

    A spectrophotometric method to determine As in tortilla and lime has been optimized, modifying the AsH{sub 3} generator. The reaction between arsin (AsH{sub 3}){sub 4} and diethyldithiocarbamate of Ag (AgDDC); was followed spectrophotometrically. The conditions under which the As remains in the ash during the calcination of the tortillas were studied. It was found that when they were heated in a quartz tube with a careful control of the air flow and oxygen, as well as the heating temperature, the arsenic loss in minimized. [Spanish] Se ha optimizado el metodo para determinar As en la tortilla y cal mediante espectrometria en el visible del color producido en la reaccion entre Arsina (AsH{sub 3}){sub 4} y dietilditiocarbamato de plata (AgDDC); modificando el generador de AsH{sub 3}. Se han buscado las condiciones en las que el arsenico permanece en las cenizas de la calcinacion de las tortillas; encontrandose que las tortillas deben calentarse en un tubo de cuarzo con control del flujo de aire y oxigeno asi como de la temperatura de calentamiento.

  5. A method for the determination of ascorbic acid using the iron(II)-pyridine-dimethylglyoxime complex

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    Arya, S. P.; Mahajan, M. [Haryana, Kurukshetra Univ. (India). Dept. of Chemistry

    1998-05-01

    A simple and rapid spectrophotometric method for the determination of ascorbic acid is proposed. Ascorbic acid reduces iron (III) to iron (II) which forms a red colored complex with dimethylglyoxime in the presence of pyridine. The absorbance of the resulting solution is measured at 514 nm and a linear relationship between absorbance and concentration of ascorbic acid is observed up to 14 {mu}g ml{sup -1}. Studies on the interference of substances usually associated with ascorbic acid have been carried out and the applicability of the method has been tested by analysing pharmaceutical preparations of vitamin C. [Italiano] Si propone un rapido e semplice metodo spettrofotometrico per la determinazione dell`acido ascorbico. L`acido ascorbico riduce il ferro(III) a ferro(II) che forma con la dimetilgliossima, in presenza di piridina, un complesso colorato in rosso. L`assorbanza della soluzione risultante e` misurata a 514 nm e si ottiene una relazione lineare tra assorbanza e concentrazione dell`acido ascorbico fino a 14 {mu}g ml{sup -1}. Si sono condotti studi sugli interferenti usualmente associati all`acido ascorbico ed e` stata valutata l`applicabilita` del metodo all`analisi di preparati farmaceutici di vitamina C.

  6. Evaluation of methods for wax determination in crude oil; Avaliacao de metodos de determinacao de parafinas em petroleo

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    Dias, Julio Cesar M.; Silva, Maria do Socorro A.J. da; Vasconcellos, Rosa C.U. [PETROBRAS S.A., Rio de Janeiro, RJ (Brazil). Centro de Pesquisas; Tamanqueira, Juliana B. [Fundacao Gorceix, Ouro Preto, MG (Brazil)

    2008-07-01

    Determining the wax content of crude oil is of great importance for petroleum industry, especially for production, storage and transportation of crude oils. Many different methodologies of wax determining are available in the technical literature. However, the selection of the most suitable method must be in accordance with the aim of the analysis and observing the specificities of each technique. The purpose of this work was to determine the performance of different techniques of wax determining applied to characterization of precipitation properties of waxy compounds in crude oils. Twelve samples of crude oils proceeding from the main Brazilian oil producing sedimentary basins were selected for this study. These samples were analyzed by three important analytical techniques of wax determining: precipitation by cooled solvent; liquid chromatography with precipitation by cooled solvent; and liquid chromatography followed by gas chromatography. Differential scanning calorimetry data related to the wax crystallization in these oils were used as parameters of validation. The results obtained in this study indicate that the liquid chromatography followed by gas chromatography method has the best performance for wax determining in crude oils. (author)

  7. Determination of polycyclic aromatic hydrocarbons (PAHs). gas chromatographic method; Determinazione degli idrocarburi policiclici aromatici (IPA). Metodo gascaromatografico

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    Menichini, E.; Viviano, G. [Istituto Superiore di Sanita`, Rome (Italy). Lab. di Igiene Ambientale

    1997-12-01

    The method enables the determination of 4- to 6- ring PAHs and particularly of carcinogenic PAHs regulated in Italy. This revision is based on the results of a national collaborative study. Sample extract, obtained by a method described in a previous report (Rapporto ISTISAN: 90/33) is cleaned up by thin layer chromatography and analysed by gas chromatography; identification is confirmed by mass spectrometry. An intralaboratory quality control program is described.

  8. Methods of Uranium Determination in solutions of Tributyl Phosphate and Kerosene; Metodos de determinacion de uranio en soluciones de fosfato de tributilo y queroseno

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    Petrement Eguiluz, J.; Palomares Delgado, F.

    1962-07-01

    A new analytical method for the determination of uranium in organic solutions of tributyl phosphate and kerosene is proposed. In this method the uranium is reectracted from the aqueous phase by reduction with cadmium in acid solution. The uranium can be determined in this solution by the usual methods. In case of very diluted solutions, a direct spectrophtometrical determination of uranium in the organic phase with dibenzoylmethane is proposed. (Author) 21 refs.

  9. An alternative method study for determining the content oils and greases derived from spectrophotometric; Estudo de um metodo alternativo para determinacao de oleos e graxas derivado do metodo espectrofotometrico

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    Moura, Leila Rose Benevides; Bezerra, Magna Angelica dos Santos [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil). Programa de Recursos Humanos da ANP, PRH-14; Melo, Josette Lourdes de Sousa; Melo, Henio Normando de Sousa [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil); Gomes, Andrea Karla Martins [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil). Dept. de Engenharia Quimica

    2004-07-01

    The determination of the Text of Oils and Greases (TOG) it can be done by several methods - gravimetrical or spectrophotometric. That work seeks to study a method alternative spectrophotometric, being compared this with the method used by Curbelo (2002). The modifications were: the reason solvent/sample, and the procedure in which the solvent the sample was mixed. For the method of Curbelo (2002) 100 mL of the sample was mixed to 10 chloroform mL and separated in separation funnel. In the proposed method, adapted denominated Chloroform, the reason was of 20 sample mL for 20 chloroform mL, being this mixture, after manual agitation, taken directly for centrifuge. The medium results were of 81,36 mg/L and 150,44 mg/L for the methods of the Chloroform and Adapted Chloroform, respectively. In spite of the medium values they present differences of almost 50%, it can be verified that the methods demonstrated certain uniformity when evaluated separately, being obtained a minimum deviation of 5,88%. With base in those preliminary results, it can be verified that the developed alternative method gets to remove more oil, mainly for more concentrated samples - exception done to the results of the pattern - and that the two methods present viability of substitution of the gravimetrical methods. (author)

  10. Spectrophotometric method for the determination of thorium in UO{sub 2} pellets; Metodo espectrofotometrico para la determinacion de torio en pastillas de UO{sub 2}

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    Acosta L, E. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)]. e-mail: eal@nuclear.inin.mx

    1995-04-15

    This report presents a procedure with the description of the spectrophotometric method for the determination of the thorium element in uranium products including powders and pellets of uranium dioxide. Quantities can be determined starting from 1 ppm. (Author)

  11. Potentiometric determination of peroxodisulfuric acid during electrolysis sulfuric acid

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    Fedor Malchik

    2013-09-01

    Full Text Available Was proposed two potentiometric methods for determining peroxodisulfuric acid during electrolysis of sulfuric acid (potentiometric titration method and direct potentiometry, based on its interaction with a known excess of a solution Fe2+.

  12. Determination of Sialic Acids by Acidic Ninhydrin Reaction

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    Yao,Kenzabroh

    1987-12-01

    Full Text Available A new acidic ninhydrin method for determining free sialic acids is described. The method is based on the reaction of sialic acids with Gaitonde's acid ninhydrin reagent 2 which yields a stable color with an absorption maximum at 470 nm. The standard curve is linear in the range of 5 to 500 nmol of N-acetylneuraminic acid per 0.9 ml of reaction mixture. The reaction was specific only for sialic acids among the various sugars and sugar derivatives examined. Some interference of this method by cysteine, cystine and tryptophan was noted, although their absorption maxima differed from that of sialic acids. The interference by these amino acids was eliminated with the use of a small column of cation-exchange resin. The acidic ninhydrin method provides a simple and rapid method for the determination of free sialic acids in biological materials.

  13. Determination of the response time of pressure transducers using the direct method; Determinacao do tempo de resposta de transdutores de pressao utilizando o metodo de medida direta

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    Perillo, S.R.P.

    1994-12-31

    The available methods to determine the response time of nuclear safety related pressure transducers are discussed, with emphasis to the direct method. In order to perform the experiments, a Hydraulic Ramp Generator was built. The equipment produces ramp pressure transients simultaneously to a reference transducer and to the transducer under test. The time lag between the output of the two transducers, when they reach a predetermined setpoint, is measured as the time delay of the transducer under test. Some results using the direct method to determine the time delay of pressure transducers (1 E Class Conventional) are presented. (author). 18 refs, 35 figs, 12 tabs.

  14. Method to determine the activity concentration and total activity of radioactive waste; Metodo para determinar la concentracion de actividad y actividad total de desechos radiactivos

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    Angeles C, A

    2001-02-15

    A characteristic system of radioactive waste is described to determine the concentration of radionuclides activity and the total activity of bundles of radioactive waste. The system this integrated by three subsystems: - Elevator of drums. - Electromechanics. - Gamma spectroscopy. In the system it is analyzed waste of issuing gamma specifically, and this designed for materials of relative low density and it analyzes materials of cylindrical recipients.

  15. Analytical Comparison of Miniaturized Methods for Selected PAH Determination in Clean Waters; Comparacion Analitica de 4 Metodos Miniaturizados de Determinacion de PAHs mediante HPLC en Aguas

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    Garcia, S.; Perez, R. M.; Fernandez, O.

    2012-04-11

    A study on the comparison and evaluation of 4 miniaturized extraction methods for the determination of selected PAHs in clear waters is presented. Four types of liquid-liquid extraction were used for chromatographic analysis by HPLC/ FD. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the scope of the methods developed at low and high levels of concentration. (Author) 13 refs.

  16. Conservative method for determination of material thickness used in shielding of veterinary facilities; Metodo conservativo para determinacao de espessura de materiais utilizados para blindagem de instalacoes veterinarias

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    Lava, Deise D.; Borges, Diogo da S.; Affonso, Renato R.W.; Moreira, Maria de L.; Guimaraes, Antonio C.F., E-mail: deise_dy@hotmail.com, E-mail: diogosb@outlook.com, E-mail: raoniwa@yahoo.com.br, E-mail: malu@ien.gov.br, E-mail: tony@ien.gov.br [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2014-07-01

    For determination of an effective method for shielding of veterinary rooms, was provided shielding methods generally used in rooms which works with X-ray production and radiotherapy. Every calculation procedure is based in traditional variables used to transmission calculation. The thickness of the materials used for primary and secondary shieldings are obtained to respect the limits set by the Brazilian National Nuclear Energy Commission (CNEN). This work presents the development of a computer code in order to serve as a practical tool for determining rapid and effective materials and their thicknesses to shield veterinary facilities. The code determines transmission values of the shieldings and compares them with data from transmission 'maps' provided by NCRP-148 report. These 'maps' were added to the algorithm through interpolation techniques of curves of materials used for shielding. Each interpolation generates about 1,000,000 points that are used to generate a new curve. The new curve is subjected to regression techniques, which makes possible to obtain nine degree polynomial, and exponential equations. These equations whose variables consist of transmission of values, enable trace all the points of this curve with high precision. The data obtained from the algorithm were satisfactory with official data presented by the National Council of Radiation Protection and Measurements (NCRP) and can contribute as a practical tool for verification of shielding of veterinary facilities that require using Radiotherapy techniques and X-ray production.

  17. Determination of Sn in 99{sup m}Tc Radiopharmaceutical Kits by Polarographic Methods; Determinacion de Estano en Radiofarmacos de 99{sup m}Tc mediante Metodos Polarograficos

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    Castro, M.; Cruz, J.; Sanchez, M.

    2009-07-01

    Kits of 99{sup m}Tc radiopharmaceuticals are used in nuclear medicine for diagnosis of different diseases. Sn (II) is one of the essential components in their formulations, which is used for reduction 99{sup m}Tc-pertechnetate in cold kits for on-site preparation 99{sup m}Tc-pertechnetate radiopharmaceuticals. Usually, these cold kits contain different additives (complexing agents, antioxidants, buffers, etc.) and the amount of Sn (II) varies from kit to kit. The determination of Sn in these products is essential in assessing their quality. We report here the development of a new polarographic method for the determination of Sn (II) and total Sn in representative radiopharmaceuticals kits (for the content of Sn and chemical composition) produced at the Center of Isotopes of Cuba (CENTIS). These methods were validated by analysis of variance and recovery techniques. From the results of the validation, the characteristic functions of uncertainties and fits are considered for the established methods, which give the necessary evidences to demonstrate the usefulness of these methods according to the current trends in Analytical Chemistry. This work provides practical results of great importance for CENTIS. After the speciation of Sn in the MAG3 radiopharmaceuticals kit is inferred that the production process is affected by uncontrolled factors that influence in the product stability, which demonstrates the necessity for analytical tools for the characterization of products and processes. (Author) 57 refs.

  18. Determination of bacterial endotoxin (pyrogen) in radiopharmaceuticals by the gel clot method. Validation; Determinacao de endotoxina bacteriana (pirogenio) em radiofarmacos pelo metodo de formacao de gel. Validacao

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    Fukumori, Neuza Taeko Okasaki

    2008-07-01

    Before the Limulus amebocyte lysate (LAL) test, the only available means of pirogenicity testing for parenteral drugs and medical devices was the United States Pharmacopoeia (USP) rabbit pyrogen test. Especially for radiopharmaceuticals, the LAL assay is the elective way to determine bacterial endotoxin. The aim of this work was to validate the gel clot method for some radiopharmaceuticals without measurable interference. The FDA's LALTest guideline defines interference as a condition that causes a significant difference between the endpoints of a positive water control and positive product control series using a standard endotoxin. Experiments were performed in accordance to the USP bacterial endotoxins test in the {sup 131}I- m-iodobenzylguanidine; the radioisotopes Gallium-67 and Thallium-201; the lyophilized reagents DTPA, Phytate, GHA, HSA and Colloidal Tin. The Maximum Valid Dilution (MVD) was calculated for each product based upon the clinical dose of the material and a twofold serial dilution below the MVD was performed in duplicate to detect interferences. The labeled sensitivity of the used LAL reagent was 0.125 EU mL{sup -1} (Endotoxin Units per milliliter). For validation, a dilution series was performed, a twofold dilution of control standard endotoxin (CSE) from 0.5 to 0.03 EU mL{sup -1}, to confirm the labeled sensitivity of the LAL reagent being tested in sterile and non pyrogenic water, in quadruplicate. The same dilution series was performed with the CSE and the product in the 1:100 dilution factor, in three consecutive batches of each radiopharmaceutical. The products {sup 131}I-m-iodobenzylguanidine, Gallium-67, Thallium-201, DTPA, HSA and Colloidal Tin were found compatible with the LAL test at a 1:100 dilution factor. Phytate and GHA showed some interference in the gel clot test. Other techniques to determine endotoxins as the chromogenic (color development) and the turbidimetric test (turbidity development), were also assessed to get

  19. Trace element determination study in human hair by neutron activation analysis; Estudo da determinacao de elementos traco em cabelos humanos pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Frazao, Selma Violato

    2008-07-01

    Human hair analysis studies have been subject of continuous interest due to the fact that they can be used as an important tool to evaluate trace element levels in the human body. These determinations have been carried out to use hair for environmental and occupational monitoring, to identify intoxication or poisoning by toxic metals, to assess nutritional status, to diagnose and to prevent diseases and in forensic sciences. Although hair analysis presents several advantages over other human tissue or fluid analyses, such as organ tissue, blood, urine and saliva, there are some controversies regarding the use of hair analysis data. These controversies arise from the fact that it is difficult to establish reliable reference values for trace elements in hair. The purpose of this study was to evaluate the factors that affect element concentrations in hair samples from a population considered healthy and residing in the Sao Paulo metropolitan area. The collected human head hair was cut in small pieces, washed, dried and analyzed by neutron activation analysis (NAA). Aliquots of hair samples and synthetic elemental standards were irradiated at the IEA-R1 nuclear research reactor for 16 h under a thermal neutron flux of about 5x10{sup 12} n cm{sup -2} s{sup -1} for As, Br, Ca, Co, Cr, Cs, Cu, Fe, K, La, Na, Sb, Sc, Se and Zn determinations. The induced gamma activities of the standards and samples were measured using a gamma ray spectrometer coupled to an hiperpure Ge detector. For quality control of the results, IAEA- 85 Human Hair and INCT-TL-1 Tea Leaves certified reference materials (CRMs) were analyzed. Results obtained in these CRMs presented for most of elements, good agreement with the values of the certificates (relative errors less than 10%) and good precision (variation coefficients less than 13.6%). Results of replicate hair sample analysis showed good reproducibility indicating homogeneity of the prepared sample. Results obtained in the analyses of dyed and

  20. An Optimised Method to Determine PAHs in a Contaminated Soil; Metodo Optimizado para la Determinacion de PAHs en un Suelo Contaminado

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    Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano castano, M. L.; Escolano Segovia, O.; Garcia Frutos, F. J.

    2007-07-20

    An analytical study is presented based on an optimised method to determine selected polycyclic aromatic hydrocarbons (PAHs) by High Performance Liquid Chromatography (HPLC) with fluorescence detection. The work was focused to obtain reliable measurements of PAH in a gas work contaminated soil and was performed in the frame of the project 'Assessment of natural remediation technologies for PAHs in contaminated soils' (Spanish Plan Nacional l+D+i, CTM 2004-05832-CO2-01): First assays were focused to evaluate an initial proposed procedure by sonication extraction in the contaminated soil. Afterwards to extend the efficiency and reduce solvent and time consuming of extraction procedures, the more relevant parameters that affect the extraction step were investigated. A comparison between sonication and microwave procedures was done, and the influence of sample grinding was studied. In general, both extraction techniques led on comparable results, although sonication procedure needs to be more carefully optimised. Finally, as a final application of the optimised method, the effect of particle size on relative distribution of selected PAHs in the contaminated soil was investigated. Relative abundance of more volatile PAHs showed a decreasing according to lower grain size, while relative abundance of less volatile compounds indicated an increasing of concentration levels for lower grain size. (Author) 10 refs.

  1. Determination of titratable acidity in white wine

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    Rajković Miloš B.

    2007-01-01

    Full Text Available The amount of titration acid in must is in the largest number of cases with in the range 5.0-8.0 g/dm3. Wines, as a rule, contain less acids than must, and according to Regulations, titratable acidity is in the range of 4.0-8.0 g/dm3 expressed in tartaric acid, because a part of tartaric acid is deposited in the form of salts (tartar or argol during alcohol fermentation. For wines that contain less than 4 g/dm3 of titratable acids there arises a suspicion about their origin, that is, that during the preparation some illegal acts were done. Because of that, the aim of this paper is to determine titratable acidity in white wine, using standard methods of determination, which are compared with the results received by potentiometric titration using ion-selective electrode. According to the received results it can be seen that wine titration with indicator gives sufficient reliable values of wine titration acidity. However, as potentiometric titration at pH value 7.00 is more reliable and objective method, the values of titratable acids content in wine, expressed through tartaric acid, are given according to this result. The analysis of differential potentiometric curves shows that these curves can give us an answer to the question of the presence of a larger amount of other nonorganic substances, which have already existed in wine. However, none of the used methods gives absolutely reliable answer what substances are present in analysed samples.

  2. Seed prepare for oil content determination by NMR method in six cotton varieties; Preparo de sementes para determinacao do teor de oleo pelo metodo de RMN em seis variedades de algodoeiro

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    Gondim-Tomaz, Rose Marry Araujo; Erismann, Norma de Magalhaes; Sabino, Nelson Paulieri; Kondo, Julio Isao; Cia, Edivaldo; Azzini, Anisio [Instituto Agronomico de Campinas, SP (Brazil). Centro de Algodao e Fibrosas Diversas]. E-mail: gondim@cec.iac.br; Soave, Daise [Instituto Agronomico de Campinas, SP (Brazil). Centro de Genetica, Biologia Molecular e Fitoquimica

    1998-07-01

    Three comparative methods (chemical seed-delinting with sulphuric acid solution, flaming and seed with linter) to prepare cotton seeds for oil determination by the Nuclear Magnetic Resonance (NMR) technique were considered. The chemical treatment with sulphuric acid was the best as long the linter interference was eliminated. The seed oil contents were determined by the NMR method in six cotton varieties from the national variety test. The IAPAR (Instituto Agronomico do Parana) 71 PR3 and IAC (Instituto Agronomico de Campinas) 20 varieties presented the highest oil content followed by the CNPA 7H, CS 50, IAC 22 and CNPA Precoce 2. (author)

  3. Spectrophotometric determination of tranexamic acid using vanillin

    Institute of Scientific and Technical Information of China (English)

    EM.A.Rind; M.G.H.Laghari; A.H.Memon; U.R.Mughal; F. Almani; N.Me-mon; M.Y.Khuhawar; M.L.Maheshwari

    2009-01-01

    A new spectrophotometric method has been examined for the determination of the tranexamic acid (TA)by derivatization with vanillin(VAN).The molar absorptivity of TA was calculated 25 160 L·mol-1·cm-1at λ max 354 nm and obeyed the Beer's law within 0.5-2.5 μg·mL-1.The color reaction was highly stable and didnot show any change in absorbance up to 24 h.The method was applied for the analysis of TA from capsules,injections and tooth pastes.The amounts of TA found in capsules,injections and tooth pastes of various pharmaceutical companies were observed with 249.0-250.9 mg/capsule,249.3-250.7 mg/injection and 0.048%-0.049%in tooth pastes with relative standard deviation(RSD)0.2%-5.0%(n=3).

  4. Determination of free fatty acids in beer.

    Science.gov (United States)

    Bravi, Elisabetta; Marconi, Ombretta; Sileoni, Valeria; Perretti, Giuseppe

    2017-01-15

    Free fatty acids (FFA) content of beer affects the ability to form a stable head of foam and plays an important role in beer staling. Moreover, the presence of saturated FAs is related sometimes to gushing problems in beer. The aim of this research was to validate an analytical method for the determination of FFAs in beer. The extraction of FFAs in beer was achieved via Liquid-Liquid Cartridge Extraction (LLCE), the FFAs extract was purified by Solid Phase Extraction (SPE), methylated by boron trifluoride in methanol, and injected into GC-FID system. The performance criteria demonstrate that this method is suitable for the analysis of medium and long chain FFAs in beer. The proposed method was tested on four experimental beers. PMID:27542484

  5. Arterial Blood Carbonic Acid Inversely Determines Lactic and Organic Acids

    OpenAIRE

    Aiken, Christopher Geoffrey Alexander

    2013-01-01

    Objective: To establish that arterial blood carbonic acid varies inversely with lactic acid in accordance with bicarbonate exchanging for lactate across cell membranes through the anion exchange mechanism to maintain the Gibbs-Donnan equilibrium.

  6. Analytical methods for 2,4-D (Dichlorophenoxyacetic acid) determination; Metodos analiticos para la determinacion del 2,4-D (Acido diclorofenoxiacetico)

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    Martinez G, M.S.M

    1999-06-01

    The 2,4-D herbicide is one of the main pesticides for controlling the bad grass in crops such as the water undergrowth. In Mexico the allowed bound of this pesticide is 0.05 mg/l in water of 2,4-D so it is required to have methods trusts and exacts, which can used in order to detected low concentration of it. In this work we show some for the conventional techniques and for establishing the 2,4-D concentrations. The UV-Vis spectrometer and liquids chromatography due that they are the most common used nowadays. Beside, we introduce a now developed technique, which is based on the neutronic activation analysis. Though use of the UV-Vis spectrometer technique it was possible target the concentrations interval between 1 and 200 mg/l. In the liquids chromatography interval was between 0.1 and 0.9, and by the neutronic activation analysis the interval was between 0.01 and 200 mg/l. (Author)

  7. Use of radioactive methods for determination of uranium, neptunium, plutonium, americium and curium isotopes in waste radioactive; Utilizacao de metodos radioanaliticos para determinacao de isotopos de uranio, netunio, plutonio, americio e curio em rejeitos radioativos

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    Geraldo, Bianca

    2012-07-01

    Activated charcoal is a common type of radioactive waste that contains high concentrations of fission and activation products. The management of this waste includes its characterization aiming the determination and quantification of the specific radionuclides including those known as Difficult-to-Measure Radionuclides (RDM). The analysis of the RDM's generally involves complex radiochemical analysis for purification and separation of the radionuclides, which are expensive and time-consuming. The objective of this work was to define a methodology for sequential analysis of the isotopes of uranium, neptunium, plutonium, americium and curium present in a type of radioactive waste, evaluating chemical yield, analysis of time spent, amount of secondary waste generated and cost. Three methodologies were compared and validated that employ ion exchange (TI+EC), extraction chromatography (EC) and extraction with polymers (ECP). The waste chosen was the activated charcoal from the purification system of primary circuit water cooling the reactor IEA-R1. The charcoal samples were dissolved by acid digestion followed by purification and separation of isotopes with ion exchange resins, extraction and chromatographic extraction polymers. Isotopes were analyzed on an alpha spectrometer, equipped with surface barrier detectors. The chemical yields were satisfactory for the methods TI+EC and EC. ECP method was comparable with those methods only for uranium. Statistical analysis as well the analysis of time spent, amount of secondary waste generated and cost revealed that EC method is the most effective for identifying and quantifying U, Np, Pu, Am and Cm present in charcoal. (author)

  8. Determination of isocyanic acid in air.

    Science.gov (United States)

    Karlsson, D; Dalene, M; Skarping, G; Marand, A

    2001-08-01

    A method is presented for the determination of isocyanic acid (ICA), HNCO, in air samples as a di-n-butylamine (DBA) derivative. The method is based on sampling in midget impinger flasks containing 10 ml of 0.01 mol l-1 DBA in toluene. Quantification was made using liquid chromatography (LC) and electrospray mass spectrometry (MS) monitoring positive ions. The instrumental detection limit for the LC-MS was 10 fmol of ICA-DBA. ICA was generated by thermal decomposition of urea. A standard solution containing the DBA derivatives of ICA was prepared by collecting the emitted ICA in an impinger flask containing DBA. ICA in the reference solution was characterised by LC and time-of-flight (TOF) MS and quantified by LC chemiluminescent nitrogen detection (LC-CLND). The instrumental detection limit for the LC-CLND was 1 ng of nitrogen. ICA was emitted during thermal degradation of PFU resins and polyurethane (PUR) lacquers, from car metal sheets. ICA was the most dominant isocyanate and in PUR coating up to 8% of the total weight was emitted as ICA and for PFU resins up to 14% was emitted as ICA. When air samples were collected in an iron foundry during casting in sand moulds with furan resins, concentrations of ICA in the range 50-700 micrograms m-3 were found in the working atmosphere. PMID:11523446

  9. Determination of acetylsalicylic acid and salicylic acid in foods, using HPLC with fluorescence detection.

    NARCIS (Netherlands)

    Venema, D.P.; Hollman, P.C.H.; Janssen, P.L.T.M.K.; Katan, M.B.

    1996-01-01

    We developed a specific and sensitive HPLC method with fluorescence detection for the determination of free acetylsalicylic acid, free salicylic acid, and free salicylic acid plus salicylic acid after alkaline hydrolysis (free-plus-bound) in foods. Acetylsalicylic acid was detected after postcolumn

  10. MERITEV PROSTANOIDOV V KRVNI PLAZMI Z METODO GC/MS

    OpenAIRE

    Lisac, Nejc

    2014-01-01

    V seminarju obravnavamo biosintezo, kemijsko zgradbo in pomen eikozanoidov v človeškem organizmu. Preučimo metodo priprave vzorca krvne plazme, postopke meritev ter kvalitativne in kvantitativne analize prostanoidov z uporabo plinskega kromatografa in masnega spektrometra. Na podlagi analize masnih spektrov z uporabo internih standardov določimo koncentracijo prisotnih prostanoidov v vzorcu.

  11. Evaluation of human dental loss caused by carbamide peroxide bleacher compared with phosphoric acid conditioning - radioactive method; Avaliacao da perda dental humana com o uso do clareador peroxido de carbamida comparado ao condicionamento com acido fosforico - metodo radiometrico

    Energy Technology Data Exchange (ETDEWEB)

    Adachi, Eduardo Makoto; Yousseff, Michel Nicolau [Sao Paulo Univ., SP (Brazil). Faculdade de Odontologia. Dept. de Dentistica; Saiki, Mitiko [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil). Lab. de Analise por Ativacao Neutronica

    2002-07-01

    The radiometric method was applied to the evaluation of dental loss caused by carbamide peroxide when it is applied on the surface layers of enamel and dentin tissues. Also the dental loss caused by the etching with 37% phosphoric acid procedure used in aesthetic restoration was assessed for comparison with those results obtained. The tooth samples irradiated with a P standard in a thermal neutron flux of the nuclear reactor were placed in contact with 10% carbamide peroxide or with 37% phosphoric acid solution. The radioactivity of {sup 32} P transferred from the radioactive teeth to the bleaching gel or to etching acid was measured using a Geiger Muller detector to calculate the mass of P removed in this treatment and losses were calculated after obtaining their P concentrations. Results obtained indicated that enamel and dentin exposed to carbamide peroxide bleaching agent lose phosphorus. The extent of enamel loss was smaller than that obtained for dentin. In the case of acid etching, there was no difference between the results obtained for enamel and dentin loss. Also the dentin loss obtained after a treatment of 30 applications of 10% carbamide peroxide was the same magnitude of that one application of 37% phosphoric acid. (author)

  12. Two new methods to determine the adhesion by means of internal friction in materials covered with films; Dos nuevos metodos para determinar la adhesion mediante friccion interna en materiales recubiertos con peliculas

    Energy Technology Data Exchange (ETDEWEB)

    Colorado, H. A.; Ghilarducci, A. A.; Salva, H. R.

    2006-07-01

    Two new models are proposed to determine the adhesion energy be means of the internal friction technique (IF) in thin films layered materials. for the first method is necessary to determine enthalpy by means of the IF technique, for which the adhesion work has been determined with experimental data. In the second method are necessary to perform IF tests at constant temperature. (Author)

  13. Nitric acid uptake by sulfuric acid solutions under stratospheric conditions - Determination of Henry's Law solubility

    Science.gov (United States)

    Reihs, Christa M.; Golden, David M.; Tolbert, Margaret A.

    1990-01-01

    The uptake of nitric acid by sulfuric acid solutions representative of stratospheric particulate at low temperatures was measured to determine the solubility of nitric acid in sulfuric acid solutions as a function of H2SO4 concentration and solution temperature. Solubilities are reported for sulfuric acid solutions ranging from 58 to 87 wt pct H2SO4 over a temperature range from 188 to 240 K, showing that, in general, the solubility of nitric acid increases with decreasing sulfuric acid concentration and with decreasing temperature. The measured solubilities indicate that nitric acid in the global stratosphere will be found predominantly in the gas phase.

  14. Fluorometric determination of uric acid in bovine milk

    DEFF Research Database (Denmark)

    Larsen, Torben; Moyes, Kasey

    2010-01-01

    The primary objective of this study is to validate a new fast method for determination of uric acid in milk. The method is based on an enzymatic-fluorometric technique that requires minimal pre-treatment of milk samples. The present determination of uric acid is based on the enzymatic oxidation o...

  15. A modification of a method for phytic acid determination

    OpenAIRE

    DRAGUTIN VELICKOVIC; BILJANA VUCELIC-RADOVIC; SRDJAN BLAGOJEVIC; MIROLJUB BARAC; SLADJANA STANOJEVIC; MAJA LJUBICIC

    1999-01-01

    Several different methods for the determination of phytic acid which do not require sophisticated equipment are currently in use. These methods have been developed to measure the phytic acid content of a variety of materials, such as plant tissues, food stuffs and soils. The aim of the work was to modify the supernatant difference, macro-method developed by Erdman and Thompson1 for the determination of the phytic acid content in soybeans and soybean protein products. A micro-method was develo...

  16. Determination of the presence of hyaluronic acid in preparations containing amino acids: the molecular weight characterization.

    Science.gov (United States)

    Bellomaria, A; Nepravishta, R; Mazzanti, U; Marchetti, M; Piccioli, P; Paci, M

    2014-10-15

    Several pharmaceutical preparations contain hyaluronic acid in the presence of a large variety of low molecular weight charged molecules like amino acids. In these mixtures, it is particularly difficult to determine the concentration and the molecular weight of the hyaluronic acid fragments. In fact zwitterionic compounds in high concentration behave by masking the hyaluronic acid due to the electrostatic interactions between amino acids and hyaluronic acid. In such conditions the common colorimetric test of the hyaluronic acid determination appears ineffective and in the (1)H NMR spectra the peaks of the polymer disappear completely. By a simple separation procedure the presence of hyaluronic acid was revealed by the DMAB test and (1)H NMR while its average molecular weight in the final product was determined by DOSY NMR spectroscopy alone. The latter determination is very important due to the healthy effects of some sizes of this polymer's fragments. PMID:25078662

  17. Microscale adaptation of the potentiometric method with ion-selective electrode for the quantification of fluoride; Adaptacion a microescala del metodo potenciometrico con electrodo ion selectivo para la cuantificacion de fluoruro

    Energy Technology Data Exchange (ETDEWEB)

    Guevara Ruiz, Paulina; Ortiz Perez, Maria Deogracias [Laboratorio de Bioquimica, Facultad de de Medicina, Universidad Autonoma de San Luis Potosi, San Luis Potosi, San Luis Potosi, (Mexico)]. E-mail: mdortiz@uaslp.mx

    2009-05-15

    Similarly to other countries, ground water from Mexico is naturally polluted by fluoride. The main effects of fluoride at typical ground water concentrations are dental fluorosis, neurological deficits and reproductive disorders. In order to verify that the fluoride concentration is within the allowed guideline in Mexico (NOM 127 and 201), it is important to monitor fluoride levels in water and commercial beverages. The aim of this work is to develop a modification of the standard potentiometric method for fluoride determination in water, in order to reduce costs and amount of potentially toxic waste substances. Both methods were validated, the standard potentiometric method with the ion selective electrode and the microscale modification proposed in this paper. The methods were compared using statistic tests and graphics, followed by the comparison of 125 samples of commercial bottled water sold in the city of San Luis Potosi. Optimal results were obtained for the validation of both methods, and the microscale modification showed statistically identical results to those obtained with the standard method in all samples of bottled water. The microscale modification is a good alternative for fluoride assessment in water and beverages, and it represents a 95 % reduction of costs and chemical waste. [Spanish] En varios paises, incluido Mexico se presenta una contaminacion natural con fluoruro en agua subterranea; los principales efectos en la salud observados en poblacion expuesta a concentraciones mayores al valor permisible (que en Mexico es de 1.5 mg/L) son la fluorosis dental y esqueletica, asi como dano reproductivo y neurologico. En varios estados de la republica Mexicana, este problema es aun desconocido, de ahi la necesidad de evaluar las concentraciones de fluoruro en agua de consumo en varias comunidades. Asi, el objetivo de este trabajo es desarrollar un metodo a microescala para la determinacion de fluoruro en agua, que al reducir la cantidad de reactivo y

  18. Scienza e conoscenza: sul valore del metodo scientifico

    Directory of Open Access Journals (Sweden)

    Riccardo Luciano Appolloni

    2014-05-01

    Full Text Available L’antico problema di riconoscere una forma di conoscenza oggettivae fondata è ancora vivo; in questo scritto cercheremo di capire se la scienza moderna possa essere una forma di conoscenza tale e, quindi, privilegiata. A tal fine ci serviremo del pensiero di alcuni epistemologi e scienziati. In particolare, nel trattare il problema del valore epistemologico del metodo scientifico, non potremo esimerci dal fare i conti con l’anarchismo metodologico di Paul K. Feyerabend, verso il quale l’esito del presente articolo sarà fondamentalmente critico. A partire dai fecondi spunti di questo filosofo, tenteremo dapprima di analizzare i caratteri distintivi della scienza e del suo metodo rispetto ad altre forme di sapere; quindi, cercheremo di individuare alcuni limiti della conoscenza razionale.

  19. Spectrophotometric determination of boric acid in boron powder with curcumin

    International Nuclear Information System (INIS)

    A rapid and accurate method was needed to determine trace amounts of boric acid for quality control and specification testing of elemental boron. The reaction between boric acid and curcumin occurs at a measurable rate only when the curcumin molecule is protonated. Protonation takes place at the carbonyl groups in the presence of a strong acid and occurs completely and rapidly when sulfuric acid is added to a solution of curcumin in acetic acid. Spectrophotometric measurements were made. The extraction of boric acid from boron powder was found to be complete within 2h when either water or the diol solution was used. Whatman No. 40 cr 42 filter paper was used to obtain diol samples free of boron particles. The extraction efficiency of 2-ethyl-1,3-hexanediol was evaluated by adding 1 ml of 500 ppM aqueous boric acid and 1 drop of 10% NaOH to accurately weighed samples of boron powder. The water then was evaporated at room temperature and the samples were extracted with diol solution. The data obtained are included. The extraction efficiency also was evaluated by determining the boric acid content of boron which had been recovered from a previous extraction and boric acid determination. The determination of boric acid using curcumin is unaffected by the presence of other compounds, except for fluoride and nitrate ions. 2 tables

  20. Determination of peracetic acid and hydrogen peroxide in the mixture

    Directory of Open Access Journals (Sweden)

    Bodiroga Milanka

    2002-01-01

    Full Text Available Iodometric and permanganometric titrations were used for determination of peracetic acid and hydrogen peroxide (H2O2 in the mixture. Two procedures were described and compared. Titrations could be done in only one vessel, in the same reaction mixture, when iodometric titration of peracetic acid was continued after the permanganometric titration of H2O2, (procedure A. Peracetic acid and H2O2, as oxidizing agents, reacted with potassium iodide in an acid medium, evolving iodine. This reaction was used for the quantitative iodometric determination of total peroxide in procedure B. H2O2 reacted with potassium permanganate in acid medium, but peracetic acid did not react under the same conditions. That made possible the selective permanganometric determination of H2O2 in the presence of peracetic acid. The procedure B was performed in two titration vessels (KV=3.4% for peracetic acid, 0.6% for H2O2. The procedure A for iodometric determination of peracetic acid in one titration vessel after permanganometric titration of H2O2 was recommended (KV=2,5% for peracetic acid, 0,45% for H2O2.

  1. Determinazione dell'azoto ammoniacale: metodo spettrofotometrico in assorbimento molecolare

    OpenAIRE

    Tartari, Gabriele A.

    2012-01-01

    Metodo analitico interno al laboratorio di idrochimica del CNR-ISE di Verbania per la determinazione dell'azoto ammoniacale. In presenza del catalizzatore sodio nitroprussiato lo ione ammonio reagisce con il gruppo fenolico del sodio salicilato; l'azione ossidante del sodio dicloro isocianurato porta alla formazione del composto blu indofenolo il cui spettro presenta un massimo di assorbanza alla lunghezza d'onda di 695 nm.

  2. Determinazione del fosforo: metodo spettrofotometrico in assorbimento molecolare

    OpenAIRE

    Tartari, Gabriele A.

    2012-01-01

    Metodo analitico interno al laboratorio di idrochimica del CNR-ISE di Verbania per la determinazione del fosforo reattivo al molibdato. L'ortofosfato reagisce con l'ammonio molibdato ed il potassio antimonio tartrato con formazione del complesso antimonio fosfomolibdico, a sua volta ridotto dall'acido L-ascorbico al colorante blu di molibdeno il cui spettro di assorbimento presenta il massimo di assorbanza a 890 nm.

  3. Analytical method of Kr-85 determination, using cryogenic concentration and separation and liquid scintillation counting; Desarrollo del metodo de concentracion y se paracion criogenica cromatografica y medida radiactiva por centelleo liquido de Kr-85

    Energy Technology Data Exchange (ETDEWEB)

    Heras, M. C.; Perez, M. M.; Grau, A.

    1983-07-01

    The method used in the Laboratory of the JEN for the determination of Kr-85 levels in gaseous effluents of nuclear power and in the atmosphere is described. Samples of air, collected in metallic cylinders, are introduced into a gas-solid chromatographic separation system which resolves Kr from the other air components. The separated Kr ia dissolved in a toluene based scintillation cocktail, and the Kr-85 content is determined by liquid scintillation counting. (Author)

  4. The two means method for the attenuation coefficient determination of archaeological ceramics from the North of Parana; Metodo dos dois meios para a determinacao do coeficiente de atenuacao de ceramicas arqueologicas do norte do Parana

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Richard Maximiliano Cunha e

    1997-12-31

    This work reports an alternative methodology for the linear attenuation coefficient determination ({mu} {rho}) of irregular form samples, in such a way that is not necessary to consider the sample thickness. With this methodology, indigenous archaeological ceramics fragments from the region of Londrina, north of Parana, were studied. These ceramics fragments belong to the Kaingaing and Tupiguarani traditions. The equation for the {mu} {rho} determination employing the two mean method was obtained and it was used for {mu} {rho} determination by the gamma ray beam attenuation if immersed ceramics, by turns, in two different means with known linear attenuation coefficient. By the other side, {mu} theoretical value was determined with the XCOM computer code. This code uses as input the ceramics chemistry composition and provides an energy versus mass attenuation coefficient table. In order to validate the two mean method validation, five ceramics samples of thickness 1.15 cm and 1.87 cm were prepared with homogeneous clay. Using these ceramics, {mu} {rho} was determined using the attenuation method, and the two mean method. The result obtained for {mu} {rho} and its respective deviation were compared for these samples, for the two methods. With the obtained results, it was concluded that the two means method is good for the linear attenuation coefficient determination of materials of irregular shape, what is suitable, specially, for archaeometric studies. (author) 25 refs., 29 figs., 28 tabs.

  5. A Simple Analytical Method Using HPLC with Fluorescence Detection to Determine Selected Polycyclic Aromatic Compounds in Filter Samples; Metodo Analitico Sencillo para la Determinacion de Compuestos Aromaticos Policiclicos en Muestras de Filtros mediante HPLC con Detector de Fluorescencia

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, S.; Perez, R. M.

    2014-06-01

    A study on the comparison and evaluation of a miniaturized extraction method for the determination of selected PACs in sample filters is presented. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the intermediate precision. (Author)

  6. Two media method for linear attenuation coefficient determination of irregular soil samples; Metodo dos dois meios para a determinacao do coeficiente de atenuacao linear de amostras irregulares de solos

    Energy Technology Data Exchange (ETDEWEB)

    Vici, Carlos Henrique Georges

    2004-07-01

    In several situations of nuclear applications, the knowledge of gamma-ray linear attenuation coefficient for irregular samples is necessary, such as in soil physics and geology. This work presents the validation of a methodology for the determination of the linear attenuation coefficient ({mu}) of irregular shape samples, in such a way that it is not necessary to know the thickness of the considered sample. With this methodology irregular soil samples (undeformed field samples) from Londrina region, north of Parana were studied. It was employed the two media method for the {mu} determination. It consists of the {mu} determination through the measurement of a gamma-ray beam attenuation by the sample sequentially immersed in two different media, with known and appropriately chosen attenuation coefficients. For comparison, the theoretical value of {mu} was calculated by the product of the mass attenuation coefficient, obtained by the WinXcom code, and the measured value of the density sample. This software employs the chemical composition of the samples and supplies a table of the mass attenuation coefficients versus the photon energy. To verify the validity of the two media method, compared with the simple gamma ray transmission method, regular pome stone samples were used. With these results for the attenuation coefficients and their respective deviations, it was possible to compare the two methods. In this way we concluded that the two media method is a good tool for the determination of the linear attenuation coefficient of irregular materials, particularly in the study of soils samples. (author)

  7. Determination of rare earth and uranium in reference biological materials certified by the method of neutron activation analysis; Determinacao de terras raras e de uranio em materiais biologicos de referencia certificados pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Lais H.P.; Saiki, Mitiko, E-mail: laispaciulli@gmail.com, E-mail: mitiko@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    The objective of this study was to evaluate the precision and accuracy of the determinations of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and U in certified reference materials (CRMs). To solve the problem of interference from fission products of U in the determination of lanthanides were obtained correction factors for this interference for {sup 140}La, {sup 141}Ce, {sup 143}Ce, {sup 153}Sm and {sup 147}Nd. The experimental procedure of Neutron Activation Analysis consisted of irradiating aliquots of each of the CRMs with synthetic standards of elements under thermal neutron flux of the IEA-R1 nuclear reactor, followed by gamma-ray spectrometry using a high-resolution hyperpurity GE detector. The analyzes of CRMs indicate good accuracy and precision of results, demonstrating the feasibility of applying of established procedure in NAA of elements studied in organic vegetable matrices.

  8. Study of the precision and trueness of the Brazilian method for ethanol and gasoline determination; Estudo da precisao e exatidao do metodo brasileiro para determinacao de etanol e gasolina

    Energy Technology Data Exchange (ETDEWEB)

    Zucchini, Ricardo R.; Hinata, Patricia [Instituto de Pesquisas Tecnologicas (IPT), Sao Paulo, SP (Brazil); Gioseffi, Carla S.; Franco, Joao B.S. [Instituto Brasileiro de Petroleo, Gas e Biocombustiveis (IBP), Rio de Janeiro, RJ (Brazil); Nascimento, Cristina R.; Torres, Eduardo S. [Agencia Nacional do Petroleo, Gas Natural e Biocombustiveis (ANP), Rio de Janeiro, RJ (Brazil)

    2008-07-01

    The determination of repeatability and reproducibility standard deviations of an analytical method, s{sub r} and s{sub R}, obtained by Interlaboratory program, makes it possible to calculate many kinds of precision limits of the method, which are needed in every laboratory's routine result comparisons and also in between-laboratories comparisons. This paper presents the results of the first interlaboratory trial, accomplished in the Brazilian petroleum sector, performed to define the trueness and precision of the Brazilian standard method for the determination of fuel anhydrous ethylic alcohol content in gasoline, that was performed by 34 experienced laboratories. The r and R values were 0,7 and 2,3 and main factors that would improve and optimize the method are presented. (author)

  9. Contribution to the spectrographic determination of impurities in uranium by the carrier distillation method; Nuevas aportaciones a la determinacion espectrografica de impurezas en materiales de uranio por el metodo de distilacion fraccionada con portador

    Energy Technology Data Exchange (ETDEWEB)

    Capdevila, C.

    1967-07-01

    The carrier distillation method for the determination of impurities in uranium has been modified in order to get a greater sensitivity. Electrodes 9.5 mm. diam. with a crater 7 mm. diam. and 10 mm. deep have been used, being the weigh of charge 300 mg.. The elements considered were: Al, As, B, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, P, Pb, Si, Sn, Ti and V, over the range 0.01 to 30 ppm. (Author) 13 refs.

  10. Semi-empirical determination of the diffusion coefficient of the Fricke Xylenol Gel dosimeter through finite difference methods; Determinacao semi-empirica do coeficiente de difusao do dosimetro Fricke Xilenol Gel atraves do metodo de diferencas finitas

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, E.O.; Oliveira, L.N., E-mail: lucas@ifg.edu.br [Instituto Federal de Educacao, Ciencia e Tecnologia de Goias (IFG), Goiania, GO (Brazil)

    2014-11-01

    Partial Differential Equations (PDE) can model natural phenomena, such as related to physics, chemistry and engineering. For these classes of equations, analytical solutions are difficult to be obtained, so a computational approach is indicted. In this context, the Finite Difference Method (FDM) can provide useful tools for the field of Medical Physics. In this study, is described the implementation of a computational mesh, in order to be used in determining the Diffusion Coefficient (DC) of the Fricke Xylenol Gel dosimeter (FXG). The initial and boundary conditions both referred by experimental factors are modelled in FDM, thus making a semi-empirical study in determining the DC. Together, the method of Reflection and Superposition (SRM) and the analysis of experimental data, served as first validation for the simulation. Such methodologies interface generated concordant results for a range of error of 3% in concentration lines for small times when compared to the analytical solution. The result for the DC was 0.43 mm{sup 2} /h. This value is in concordance with measures parameters range found in polymer gels dosimeters: 0.3-2.0 mm{sup 2} /h. Therefore, the application of computer simulation methodology supported by the FDM may be used in determining the diffusion coefficient in FXG dosimeter. (author)

  11. Drawing up of a procedure for vanadium determination in mussels using the neutron activation analysis method; Estabelecimento de procedimento para determinacao de vanadio em mexilhoes pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Seo, Daniele, E-mail: danyseo@uol.com.b [Universidade Presbiteriana Mackenzie, Sao Paulo, SP (Brazil). Centro de Ciencias Biologicas e da Saude; Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Vasconcellos, Marina B.A.; Saiki, Mitiko; Catharino, Marilia G.M.; Moreira, Edson G., E-mail: mbvascon@ipen.b, E-mail: mitiko@ipen.b, E-mail: mgcatharino@uol.com.b, E-mail: emoreira@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Sousa, Eduinetty C.P.M. de; Pereira, Camilo D.S., E-mail: edvinett@usp.b, E-mail: camilo.pereira@usp.b [Universidade de Sao Paulo (IO/USP), SP (Brazil). Inst. Oceanografico. Lab. de Ecotoxicologia Marinha

    2009-07-01

    This work establishes an adequate procedure for obtaining reliable results for determination of vanadium in mussels, leg by leg by the neutron activation analysis (NAA), viewing the posterior application on the bio monitoring the coastal pollution, particularly near the petroleum terminals.For the evaluation of result quality concerning to the quality of those results, the work analysed the reference material certification NIST SRM 1566b Oyster Tissue. The precision of the results were also analysed using repetitions of mussel samples collected at the coastal of northern Sao Paulo state, Brazil. The NAA procedure consisted of 200 mg of sample and a synthetic standard of vanadium during a period of 8 s and under a thermal neutron flux of 6.6 x 10{sup 12} n cm{sup -2} s{sup -1} at the pneumatic station 4 of the IEA-R1 nuclear reactor of IPEN-CNEN/SP. After a 3 min decay, the measurements of the gamma activities of the sample and the standard were done using a Ge hyper pure semi-conductor detector, connected to gamma ray multichannel analyser. The vanadium were determined by the measurement of the gamma activity of the {sup 52}V through the 1434.08 keV peak, and half-life time of 3.75 min. The concentration of V were calculated by the comparative method. The obtained results indicated the viability of the NAA procedure established for the determination of vanadium in mussels

  12. A method for the determination of D(-)-lactic acid

    NARCIS (Netherlands)

    Hamer, C.J.A. van den; Elias, R.W.

    1958-01-01

    A method for the determination of D(—)-lactic acid is described. An acetone powder from Escherichia coli B in the presence of methylene blue oxidizes D(—)-lactic specifically. Oxygen consumption in a Warburg apparatus was used as a measure of the D(—)-lactic acid.

  13. Analysis of a calculation method for the determination of the value of safety or control bars; Analisis de un metodo de calculo para la determinacion del valor de barras de seguridad o control

    Energy Technology Data Exchange (ETDEWEB)

    Aguilar H, F.; Torres A, C.; Filio L, C. [ININ, Gcia. de Reactores, 52045 Ocoyoacac, Estado de Mexico (Mexico)

    1982-09-15

    Due to the control or safety bars in a nuclear reactor are constituted by strongly absorbent materials, the Diffusion Theory like tool for the calculation of bar values is not directly applicable, should it use the Transport Theory. However the speed and economy of the Diffusion codes for the reactors calculation, those make attractiveness and by this reason its are used in the determination of characteristic parameters and even in the determination of bar values, not without before to make some theoretical developments that allow to make applicable this theory. The application of the Diffusion Theory in strongly absorbent media is based on the use of some effective cross sections distinct from the real ones obtained when imposing the reason that among the flow and it gradient in the external surface of such media (control element in general, bar type or flagstone) be similar to the one obtained using Transport Theory in all the control region (multiplicative and absorbent media) with those real cross sections. The effective cross sections were obtained of the Leopard-NUMICE cell code which has incorporate the respective calculation theory of effective cross sections. Later these constants its were used in the bidimensional diffusion code Exterminator-II, simulating in it, the distribution of safety or control bars. From the cell code its were also obtained the respective constants of the homogeneous fuel cell. The results as soon as those obtained bar values of the diffusion code, its were compared with some experimental results obtained in the R{phi} Swedish reactor of natural uranium and heavy water. In this work an analysis of the bar value of one of them, trying to determine the applicability of the method is made. (Author)

  14. Preliminary studies for the determination of alpha emitters using the gross alpha coprecipitation methods; Estudios preliminara para la determinacion de emisores alfa mediante el metodo de coprecipitationd e alfa total

    Energy Technology Data Exchange (ETDEWEB)

    Suarez-Navarro, J. A.; Pujol, L.; Suarez, J. A.; Pablo, M. A. de

    2003-07-01

    The radiological quality of drinking water in Spain is regulated by Nuclear Security Guideline No, 7.7 (Rev.1) of the Nuclear Security Council (NSC). this guideline establishes the protocol to follow when the radiological level exceeds 0,1 Bq.l''1. When this level is passed, the responsible alpha emitter must be identified; ''210 Po, ''226Ra, ''230Th, ''239Pu, ''224Ra, ''234 U and ''138 U. Activity due to these isotopes is usually determined using alpha spectrometry with semiconductor detectors. This method allows the activity of the alpha emitters to be determined with a good sensitivity. however, it requires long radiochemical isolations and long counting times, so the method is not suitable for rough estimate radiological analysis. In this preliminary work, we present the conditioning of the sample-precipitate that is essential for further radiochemical isolations. (Author) 9 refs.

  15. Determination of L- Ascorbic Acid in Plasma by Voltammetric Method

    OpenAIRE

    Behfar, Abdol Azim; Sadeghi, Nafiseh; Jannat, Behrooz; Oveisi, Mohammad Reza

    2010-01-01

    Voltammetric techniques have been considered as important methods among the analytical techniques used for the identification and determination of trace concentrations of many biological molecules such as L-ascorbic acid (AA). L-ascorbic acid is an electro-active molecule, though it is difficult to determine its value directly with a majority of electrodes made of carbon and transition metals, because of electrode surface problems. The present study is based on I-E curves for AA analysis at v...

  16. Analytical Evaluation to Determine Selected PAHs by HPLC in a Type 2 Fuel; Evaluacion Analitica de 4 Metodos de Determinacion de PAHs medianteHPLC en un Fuel de Tipo II

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano Castano, M. L.; Escolano Segovia, O.; Garcia Frutos, F. J.

    2009-05-21

    An evaluation of analytical parameters to determine selected PAHs in a fuel oil type II by HPLC coupled to fluorescence and diode detectors is presented. The study was focused on four conventional treatments of these kinds of oil samples and the main objective was giving a measure of confidence level of PAH results in the fuel oil. This study was performed in the frame of the project Assessment of natural attenuation of PAHs in agricultural soil contaminated with fuel from an accidental spill (Spanish National Plain I+D+I, CTM2007-64537). This paper is presented as follows: Analysis of reference material 1582 (NIST) by using the four kinds of sample treatments of interest. Application of variance analysis to compare results obtained from type II fuel by using each sample treatment and chromatographic detector. Finally, a statistic calculation was performed to measure uncertainty components in chromatographic analysis. (Author)

  17. Determination of viscosity of fayalite slags for kv model and measurements by means of inclined plane; Estimacion de la viscosidad de escorias fayaliticas utilizando el modelo de calculo kv y el metodo experimental del plano inclinado

    Energy Technology Data Exchange (ETDEWEB)

    Bazan, V.; Goni, C.; Castella, L.; Brandaleze, E.; Verdeja, L. F.; Parra, R.

    2006-07-01

    The viscosity of the lands represents one of the most relevant variables of most of the processes metallurgical and kinetics of the refine operations, since it is one of the decisive factors of the efficiency in the reactions between metal and lag, as much as slag-refractory. In the last decades, the mathematical models of different metallurgical processes have established methods to predict viscosity of mixtures of oxides fused to high temperatures in function of the chemical composition. The model developed by Toguri, based on the data reported by Johasen and Winterhager et al has proposed the Kv model. The used index it is similar to the relationship used in the steel industry like the basicity index. It is presented in this work values determined of viscosity in experimental form by means of the technique of inclined plane. (Author)

  18. Uncertainty Evaluation and Influence of Gran Size to Determine PAHs in a Contaminated Soil; Influencia del Tamano de Particula de un Suelo Contaminado en las Incertidumbres Asociadas al Metodo de Determinacion de PAHs

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Escolano Segoviano, O.; Garcia Frutos, F. J.

    2007-07-20

    An evaluation of uncertainty associated to PAH determination in a contaminated soil is presented. The work was focused to measure the influence of grain size on concentration deviations and give a measure of result confidence of PAHs in the gasworks contaminated soil. This study was performed in the frame of the project 'Assessment of natural remediation technologies for PAHs in contaminated soils'(Spanish Plan Nacional I+D+i, CTM 2004-05832-CO2-01). This paper is presented as follows: A brief introduction which describes the main uncertainty contributions associated to chromatographic analysis. Afterwards, a statistic calculation was performed to measure each uncertainty component. Finally, a global uncertainty was calculated and the influence of grain size and distribution of compounds according to volatility was evaluated. (Author) 10 refs.

  19. Analytical Evaluation to Determine Selected PAHs in a Contaminated Soil With Type II Fuel; Metodo Optimizado de Extraccion por Ultrasonidos para la Determinacion de PAHs Seleccionados en un Suelo Contaminado con Fuel de Tipo II

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano Castano, M. L.; Garcia Frutos, F. J.

    2010-10-21

    A study on the optimization of an ultrasonic extraction method for selected PAHs determination in soil contaminated by type II fuel and by using HPLC with fluorescence detector is presented. The main objective was optimize the analytical procedure, minimizing the volume of solvent and analysis time and avoiding possible loss by evaporation. This work was carried out as part of a project that investigated a remediation process of agricultural land affected by an accidental spillage of fuel (Plan Nacional I + D + i, CTM2007-64 537). The paper is structured as: Optimization of wavelengths in the chromatographic conditions to improve resolution in the analysis of fuel samples. Optimization of the main parameters affecting in the extraction process by sonication. Comparison of results with those obtained by accelerated solvent extraction. (Author) 3 refs.

  20. Evaluation of analyte additions method for sodium determination in fuel ethanol by flame atomic emission spectrometry; Avaliacao do metodo das adicoes de analito para a determinacao de sodio em alcool combustivel por espectrometria de emissao atomica em chama

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Adriana Paiva de; Okumura, Leonardo Luiz; Gomes Neto, Jose Anchieta [UNESP, Araraquara, SP (Brazil). Inst. de Quimica. Dept. de Quimica Analitica

    2002-07-01

    The analyte additions method was applied for sodium determination in fuel ethanol by atomic emission spectrometry. Graphics involving emission intensity versus analyte concentration in the 0 - 0.300 mg Na L{sup -1} interval concentration range containing 2.1 g K L{sup -1} as an ionisation buffer. Twenty samples of commercial fuel ethanol were collected in different gas stations located in Araraquara city, analyzed and results obtained varied from 0.0072 to 1.55 mg Na L{sup -1}. The limits of detection (L.O.D.) varied from 0.0026 to 0.0239 mg Na L{sup -1}. Recoveries varied in the 95 - 104 % interval. The relative standard deviations (n=12) for three analyte additions in all samples were {<=}4,1 %. (author)

  1. Determinants of folic acid knowledge and use among antenatal women.

    LENUS (Irish Health Repository)

    McDonnell, R

    1999-06-01

    Although recommendations on folic acid use were issued by health authorities in a number of countries in the early 1990s, uptake of peri-conceptional folic acid is still disappointingly low. Regardless of food fortification policies, folic acid promotion will probably be required in most countries to optimize folate levels among women of child-bearing age. The aim of this study was to examine folic acid knowledge and use, and their determinants among antenatal women in the east of Ireland in 1997.

  2. Separation and determination of some carboxylic acids by capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Sladkov, V.; Fourest, B

    2006-07-01

    Separation and determination of some organic acids, mono-carboxylic (formic and acetic), dicarboxylic (oxalic and tartaric), tricarboxylic (citric) acids and aromatic acids (phtalic, benzoic, mellitic and trimellitic), by capillary electrophoresis are reviewed. The method development parameters, such as separation and injection mode, are discussed. Special attention is paid to the comparison of different detection types (spectroscopic and electrochemical). The optimisation of the carrier electrolyte composition (choice of carrier electrolyte, effect of pH, ionic strength, electro-osmotic flow modifier) is treated. Different additives (alkali-earth and transition metal ions, cyclodextrins and alcohol), which are often used for improving organic acid separation, are also considered. (authors)

  3. Separation and determination of some carboxylic acids by capillary electrophoresis

    International Nuclear Information System (INIS)

    Separation and determination of some organic acids, mono-carboxylic (formic and acetic), dicarboxylic (oxalic and tartaric), tricarboxylic (citric) acids and aromatic acids (phtalic, benzoic, mellitic and trimellitic), by capillary electrophoresis are reviewed. The method development parameters, such as separation and injection mode, are discussed. Special attention is paid to the comparison of different detection types (spectroscopic and electrochemical). The optimisation of the carrier electrolyte composition (choice of carrier electrolyte, effect of pH, ionic strength, electro-osmotic flow modifier) is treated. Different additives (alkali-earth and transition metal ions, cyclodextrins and alcohol), which are often used for improving organic acid separation, are also considered. (authors)

  4. Subsurface microbial ecology. Epi fluorescence direct counts; Ecologia microbica del sottosuolo: metodo di conta diretta in epifluorescenza

    Energy Technology Data Exchange (ETDEWEB)

    Barra Caracciolo, A.; Silvestri, C.; Creo, C.; Izzo, G. [ENEA, Centro Ricerche Casaccia, Rome (Italy). Dipt. Ambiente

    1998-07-01

    To the aim of recognize the importance of microorganisms in affecting or even determining the fate of xenobiotics in the subsurface environment evaluating bacteria concentration in a subsurface ecosystem, the report discusses a soil sample treatment method which has been developed for epi fluorescence direct counting with DAPI. [Italian] Lo studio discute un metodo di trattamento del campione per la conta diretta in epifluorescenza con un marcatore selettivo per il DNA, il DAPI, al fine di quantificare la concentrazione batterica del sottosuolo e studiare il ruolo dei microrganismi nella biodegradazione delle molecole esogene, ancora poco indagato.

  5. Experimental determination of prompt neutron decay constant of IPEN/MB-01 reactor by Rossi-{alpha} method; Determinacao experimental da constante de decaimento de neutrons prontos do reator IPEN/MB-01 via o metodo Rossi-{alpha}

    Energy Technology Data Exchange (ETDEWEB)

    Kuramoto, Renato; Santos, Adimir dos; Jerez, Rogerio; Bitelli, Ulysses D' Utra; Diniz, Ricardo; Madi, Tufic [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)]. E-mail: ryrkuram@ipen.br

    2005-07-01

    One major objective of this work is to experimentally estimate the prompt neutron decay constant, {alpha}, on the IPEN/MB-01 research reactor at Sao Paulo. In order to achieve our goal, we will use a microscopic noise technique called Rossi-{alpha} method. This method is based on the statistical nature of the fission-chain process. Using a coincidence acquisition system, the rationale is to experimentally determine the probability distribution of detecting neutrons from the same chain. Through a leastsquares fit of this distribution we estimate {alpha}=({beta}{sub eff}-{rho})/{lambda}. The {alpha} parameter will be measured for different sub-critical levels, and the ratio {beta}{sub eff}/{lambda} is obtained via extrapolation to {rho}=0. A specific acquisition system for Rossi-{alpha} measurements has been developed in order to achieve our objective. This system is based on a multichannel scaler controlled by virtual instruments that records the timing of all neutron events, allowing data analysis during the acquisition. The first measurements were performed using one BF{sub 3} detectors positioned at the center of the core of IPEN/MB-01 research reactor. In this work we will present a preliminary set of Rossi-{alpha} measurements performed on the IPEN/MB-01 research reactor at Sao Paulo. (author)

  6. Voltammetric determination of uric acid by using gold nanotubule electrode

    Institute of Scientific and Technical Information of China (English)

    Yue Rong Wang; Ping Hu; Qiong Lin Liang; Guo An Luo; Yi Ming Wang

    2007-01-01

    Gold nanotubule membranes were prepared by using electroless deposition of gold within the pores and surfaces of polycarbonate track-etched membranes. And the gold nanotubule membrane was used as an electrode for determination of uric acid in urine samples for the first time. In Britton-Robinson buffer of pH 4.56, uric acid exhibited well-defined differential pulse voltammograms. And the interference between coexistent ascorbic acid and uric acid was overcome owing to the attractive ability of the gold nanotubule electrode to yield a large anodic peak difference ca. 0.404 V (vs. SCE). The proposed method was then applied to the determination of uric acid in urine without any pretreatment.

  7. Determination of chlorogenic acid by flow injection irreversible biamperometry

    Institute of Scientific and Technical Information of China (English)

    Li Jun Li; Qi Feng Chen; Lai Bo Yu; Zhao Heng Zhong; Jun Feng; Hao Cheng; Hong Xing Kong; Jian Ling Wu

    2007-01-01

    A flow injection irreversible biamperometric method for the determination of chlorogenic acid is described. The proposed method is based on the electrochemical oxidation of chlorogenic acid at pretreated platinum electrode and the reduction of permanganate at another electrode to form an irreversible biamperometric detection system. Under the external potential difference(△E) of 0 V, in the 0.05 mol/L sulfuric acid, chlorogenic acid can be determined over the range 0.8-120 mg/L with a sample measurement frequency of 80 samples/h. The detection limit is 0.18 mg/L. The proposed method exhibits the satisfactory reproducibility with a relative standard derivation (R.S.D.) of 2.21% for 19 successive determinations of 40 mg/L.

  8. [Spectrophotometric determination of aromatic amino compounds with J-acid].

    Science.gov (United States)

    Yin, Xiao-hang; Shi, Wen-jian; Shen, Xin; Ma, Jun-tao; Li, Liang

    2015-01-01

    The problems such as chromogenic reaction selectivity, reaction rate, sensitivity and water-solubility of azo compounds were considered. The molecular structures of coupling components were theoretically designed and screened in the present research The reaction conditions and methods of chromogenic reaction were investigated. J-Acid (2-amino-5-naphthol-7-sulfonic acid) as a coupling reagent to determine aromatic amino compounds was established. In the presence of potassium bromide, at room temperature, nitrite reacted with aromatic amino compounds in the medium of thin hydrochloric acid. Then diazonium salt reacted with J-Acid in the aqueous solution of sodium carbonate, forming coloured azo dye, which had a maximum adsorption at 480 nm. The molar adsorption coeffcients of aniline, 4-aminobenzene sulfonic acid and 1-naphthylamine were 3. 95 X 10(4), 3. 24 X 10(4) and 3. 91 X 10(4) L . mol-1 . cm-1 , respectively. Experimental results showed that common coexisting ions on the surface water did not affect the results of determination. J-Acid of spectrophotometry was used to determine the samples of Shanghai Fu Xing Dao canal. Meanwhile, recovery experiments by standard addition method were done. Experiment results showed that the recoveries of aniline were in the range of 98. 5%-102. 1%, and RSD was 2. 08%. J-Acid is a common organic reagent. It is soluble in water and low volatile, and its toxicity is much lower than N-ethylenediamine. spectrophotometric determination of aromatic amino compounds by J-Acid has the advantage of high sensitivity, good selectivity, simple rapid operation and accurate results, and thus it can be used for the determination of trace aromatic amino compounds in the environmental water.

  9. PRIPRAVA IN KARAKTERIZACIJA BAKROVIH SELENIDOV S SONOKEMIJSKO METODO

    OpenAIRE

    Košiček, Blaž

    2012-01-01

    Sonokemija je izraz za aplikacijo ultrazvočnih valov na kemijskih reakcijah. Ukvarja se z razumevanjem efekta zvočnih valov na kemijske sisteme, vendar za kemika zvok po vsej verjetnosti ne bi bil prva izbira oblike energije za stimulacijo kemijskih reakcij. Danes se veliko število znanstvenikov ukvarja s tem novim področjem raziskovanja. Naša raziskava je temeljila na sintezi nanokristalov bakrovih selenidov s sonokemijsko metodo. Naš cilj je bil sintetizirati nanokristale s spreminjanje...

  10. Determination of primary nitroparaffins by the nitrous acid reaction

    Energy Technology Data Exchange (ETDEWEB)

    Altshuller, A.P.; Cohen, I.R.

    1960-06-01

    The determination of nitroparaffins and particularly of primary nitroparaffins was reviewed recently. A spectrophotometric method for determining microgram quantities of primary nitroparaffins by coupling with diazotized sulfanilic acid was described. In the course of investigating the gas-phase products of olefins and nitrogen oxides, the reactions of some representative members of various classes of nitroparaffins with nitrous acid also were measured. This type of reaction goes back to the classical red, white and blue reaction of Meyer and Locher. The blue reaction of nitrous acid with secondary nitroparaffins was investigated as a colorimetric procedure. In the present work the nitrous acid reaction with primary nitroparaffins is of immediate interest, but the reactions of secondary nitroparaffins, dinitroparaffins, and a variety of nitroalcohols also are measured. 8 references, 1 table.

  11. Determination and Correlation for Solubility of Aromatic Acids in Solvents

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Solubility of benzoic acid, terephthalic acid and 2,6-naphthalene dicarboxylic acid in water, acetic acid, N,N-dimethyfformamide, N,N-dimethylacetamide, dimethyl sulphoxide and N-methyl-2-ketopyrrolidine were measured by dynamic method. The solubilities were calculated by UNIFAC group contribution method, in which new groups, BCCOOH and NCCOOH, were introduced to express the activity coefficients of aromatic acids and new interaction parameters of the new groups were expressed as the function of temperature, which were determined from the experimental data. The new interaction parameters provided good calculated result. The experimental data were also correlated with Wilson and λ-h models, and results were compared with present UNIFAC model.

  12. Determination of Ascorbic Acid in Vegetables by Derivative Spectrophotometry

    OpenAIRE

    Aydoğmuş, Zeynep; ÇETİN, Sevil Müge

    2002-01-01

    Determination of ascorbic acid (AA) in garlic, green pepper and chestnut was performed by derivative spectrophotometry without using any pre-separation or background correction techniques. The method is based on the measurement of the distances between two extremum values (peak-to-peak amplitudes) in second and third order derivative spectra of the extracts. Ten percent trichloroacetic acid was found to be the most suitable extraction solution. In the second order derivative spectru...

  13. Fluorimetric determination of pipemidinic acid using the europium chelate.

    Science.gov (United States)

    Egorova, A; Beltyukova, S; Teslyuk, O

    1999-11-01

    The sensitized luminescence of europium ion in the complexes with pipemidinic acid is investigated. It was shown that in the result of intramolecular energy transfer from ligand to lanthanide ion the luminescence intensity of the latter increases by 10(10) times. The luminescence properties of the complex were studied and the high sensitive luminescence method for the determination of pipemidinic acid has been developed.

  14. The need of alkalinity determination in the characterization of rain; Necesidad de la determinacion de la alcalinidad en la caracterizacion de la lluvia

    Energy Technology Data Exchange (ETDEWEB)

    Pal Verma, Mahendra [Instituto de Investigaciones Electricas, Cuernavaca (Mexico)

    1998-01-01

    In this paper is presented the alkalinity determination of the carbonic species in the rain waters by the Gran titration method. The alkalinity values obtained by this method in low electric conductivity waters are fairly reliable. Also, the existing studies on the characterization of acid rains, are discussed. [Espanol] En este trabajo se presenta la medicion de la alcalinidad y la determinacion de las especies carbonicas en las aguas de lluvia por el metodo de la titulacion de Gran. Los valores de alcalinidad obtenidos por este metodo en las aguas de baja conductividad electrica son bastante confiables. Asimismo, se discuten los estudios existentes sobre la caracterizacion de la lluvia acida en la republica mexicana.

  15. Individual and simultaneous determination of uric acid and ascorbic acid by flow injection analysis.

    Science.gov (United States)

    Almuaibed, A M; Townshend, A

    1992-11-01

    Flow injection methods for the individual and simultaneous determination of ascorbic acid and uric acid are proposed. A spectrophotometer and a miniamperometric detector are connected in sequence. The calibration graphs for uric acid obtained by measuring its absorbance at 293 nm and its current at +0.6 V are linear up to at least 80 and 70 mug/ml, respectively, with an rsd (n = 10) of 1 % for both methods at mid-range concentrations. The calibration graph for ascorbic acid with amperometric detection is linear up to 80 mg/l. with an rsd (n = 10) of 0.8% at 30 mg/l. The simultaneous determination of uric acid and ascorbic acid is based on measurement of the absorbance of uric acid at 393 nm and amperometric determination of both analytes at +0.6 V. The average relative errors of the analysis of binary mixtures of uric acid and ascorbic acid are 2.2 and 4.2%, respectively. PMID:18965554

  16. Potentiometric determination of free acidity in presence of hydrolysable ions and a sequential determination of hydrazine.

    Science.gov (United States)

    Ganesh, S; Khan, Fahmida; Ahmed, M K; Pandey, S K

    2011-08-15

    A simple potentiometric method for the determination of free acidity in presence of hydrolysable ions and sequential determination of hydrazine is developed and described. Both free acid and hydrazine are estimated from the same aliquot. In this method, free acid is titrated with standard sodium carbonate solution after the metal ions in solutions are masked with EDTA. Once the end point for the free acid is determined at pH 3.0, an aliquot of formaldehyde is added to liberate the acid equivalent to hydrazine which is then titrated with the same standard sodium carbonate solution using an automatic titration system. The described method is simple, accurate and reproducible. This method is especially applicable to all ranges of nitric acid and heavy metal ion concentration relevant to Purex process used for nuclear fuel reprocessing. The overall recovery of nitric acid is 98.9% with 1.2% relative standard deviation. Hydrazine content has also been determined in the same aliquot with a recovery of nitric acid is 99% with 2% relative standard deviation. The major advantage of the method is that generation of corrosive analytical wastes containing oxalate or sulphate is avoided. Valuable metals like uranium and plutonium can easily be recovered from analytical waste before final disposal. PMID:21726724

  17. Contributions te the study of methods and factors affecting the spectrophotometric determination of boron traces with carmin uranium compounds; Contribucion al estudio del metodo y factores que afectan a la determinacion espectrofotometrica de trazas de boro con Carmin en compuestos de uranio

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez Cellini, R.; Gasco Sanchez, L.

    1956-07-01

    The study of some factors affecting the spectrophotometric determination of boron traces with carmin is made; the influence of carmin from different origin, the stability of complex carmin-boric acid in relation with the sulphuric acid concentration, the interference produced by ion nitrate, and the ion uraline and light influence are discussed. (Author) 36 refs.

  18. Determination of acidity constants of enolisable compounds by capillary electrophoresis.

    Science.gov (United States)

    Mofaddel, N; Bar, N; Villemin, D; Desbène, P L

    2004-10-01

    Research on the structure-activity relationships of molecules with acidic carbon atoms led us to undertake a feasibility study on the determination of their acidity constants by capillary electrophoresis (CE). The studied molecules had diverse structures and were tetronic acid, acetylacetone, diethylmalonate, Meldrum's acid, 3-methylrhodanine, nitroacetic acid ethyl ester, pyrimidine-2,4,6-trione, 3-oxo-3-phenylpropionic acid ethyl ester, 1-phenylbutan-1,3-dione, 5,5-dimethylcyclohexan-1,3-dione and homophthalic anhydride. The p Ka range explored by CE was therefore very large (from 3 to 12) and p Ka values near 12 were evaluated by mathematical extrapolations. The analyses were carried out in CZE mode using a fused silica capillary grafted (or not) with hexadimethrine. Owing to the electrophoretic behaviour of these compounds according to the pH, their acidity constants could be evaluated and appeared in perfect agreement with the literature data obtained, a few decades ago, by means of potentiometry, spectrometry or conductimetry. The p Ka of homophthalic anhydride and 3-methylrhodanine were evaluated for the first time.

  19. Spectrophotometric determination of uranium with benzohydroxamic acid in aqueous medium

    International Nuclear Information System (INIS)

    A spectrophotometric method has been developed for the determination of uranium with benzohydroxamic acid (BHA). Uranium in the hexavalent state forms a yellowish orange colored chelate with BHA. The absorbance of the complex is maximum at pH 6.0, excluding pH7 and complex is stable for more than 72 hours. The maximum absorbance at 304 nm is considered for quantification of uranium. The present method is validated and good agreement with spectrophotometric determination of uranium with thiocyanate. Uranium in the range 1-10 μg/ml has been determined with good precision. The described method is simple, precised and accurate. It can be applied for the determination of uranium in raffinates of Purex process, without producing the nuclear waste in organic phase

  20. Vitamin B2 content determination in liver paste by using acid and acid-enzyme hydrolysis

    Directory of Open Access Journals (Sweden)

    Basić Zorica

    2007-01-01

    Full Text Available Background/Aim. Vitamin B2 is available in foodstuff in the form of coenzyme and in free form. For its content determination a few procedures should be performed (deliberation from a complex, extraction of free and deliberated form and detection, identification and quantification. There is a particular problem in determination of vitamin B2 in the meat products. For a determination of total vitamin B2 content in liver paste two preparation procedures are compared: acid and acid-enzymatic hydrolysis. The aim of this study thus, was to compare the effectiveness of these two different procedures for vitamin B2 content determination in liver paste. Methods. High pressure liquid chromatography (HPLC method with fluorescence detector, as specific and adequately sensitive for the foodstuff of a complex composition with a natural vitamin content, was used for determination of vitamin B2 in liver paste. Acid hydrolysis was performed with the application 0.1 M hydrochloric acid in a pressure cooker, and enzymatic hydrolysis was performed with the 10% takadiastase on 45 ºC within four hours. Ten samples of liver paste from the supply of the Serbian Army were examined. Separation was performed on the analytical column Nucleosil 50−5 C18 with mobile phase 450 ml CH3OH + 20 ml 5 mM CH3COONH4, and detection on the fluorescent detector with the variable wave length. Both methods were validated: examining a detection limit, quantification limit, specificity (because of a possible B2 vitamin interference with reagents, linearity of a peak area and standard concentration of B2 vitamin ratio in the range from 0.05 μg/ml to 2 μg/ml, precision for the 0.05 μg/ml concentration and recovery. Results. All the previously examined parameters validated both methods as specific, precise and reproductive, with a high recovery (98.5% for acid and 98.2% for acid - enzymatic hydrolysis, as well as linearity in a range that significantly superseded the expected content in

  1. Easy modification of glassy carbon electrode for simultaneous determination of ascorbic acid, dopamine and uric acid.

    Science.gov (United States)

    Thiagarajan, Soundappan; Tsai, Tsung-Hsuan; Chen, Shen-Ming

    2009-04-15

    A glassy carbon electrode (GCE) has been modified by electrochemical oxidation in mild acidic media (0.1 mol l(-1) H(2)SO(4)) and could be applied for individual and simultaneous determination of ascorbic acid (AA), dopamine (DA) and uric acid (UA). Oxidized GCE shows a single redox couple (E(0)'=-2.5 mV) which is based on the formation functional groups during the electrochemical pretreatment process. Proposed GCE successfully decreases the over potentials for the oxidation process of these species (AA, DA and UA) comparing with bare GCE. The oxidized GCE has its own simplicity, stability, high sensitivity and possesses the potential for simultaneous determination of AA, DA and UA. PMID:19162467

  2. Simultaneous determination of salicylic acid and salicylamide in biological fluids

    Science.gov (United States)

    Murillo Pulgarín, J. A.; Alañón Molina, A.; Sánchez-Ferrer Robles, I.

    2011-09-01

    A new methodology for the simultaneous determination of salicylic acid and salicylamide in biological fluids is proposed. The strong overlapping of the fluorescence spectra of both analytes makes impossible the conventional fluorimetric determination. For that reason, the use of fluorescence decay curves to resolve mixtures of analytes is proposed; this is a novel technique that provides the benefits in selectivity and sensitivity of the fluorescence decay curves. In order to assess the goodness of the proposed method, a prediction set of synthetic samples were analyzed obtaining recuperation percentages between 98.2 and 104.6%. Finally, a study of the detection limits was done using a new criterion resulting in values for the detection limits of 8.2 and 11.6 μg L -1 for salicylic acid and salicylamide respectively. The validity of the method was tested in human serum and human urine spiked with aliquots of the analytes. Recoveries obtained were 96.2 and 94.5% for salicylic acid and salicylamide respectively.

  3. Polarographic determination of metyrosine through treatment with nitrous acid.

    Science.gov (United States)

    Aly, F A; Belal, F; el-Brashy, A

    1993-10-15

    A simple and sensitive polarographic method is described for the determination of metyrosine through treatment with nitrous acid. The different experimental parameters affecting the derivatization process, as well as the polarographic analysis were studied. The derivatization product was found to be reducible at the dropping mercury electrode over the whole pH range in Britton Robinson buffers. At pH 5, a well-defined diffusion-controlled cathodic wave was produced. The limiting current versus the concentration plot was linear over the range 8-80 mumol/l in the direct current mode with a detection limit of 0.2 mumol/l. The method was then applied to the determination of metyrosine capsules, and the results obtained were in good agreement with those given by the USP method.

  4. Diagnostic value of prostatic acid phosphatase as determined by radioimmunoassay

    International Nuclear Information System (INIS)

    Serum concentrations of prostatic acid phosphatase (PAP) were determined with 4 different radioimmunoassays and with the standard enzymatic method (p-nitrophenylphosphate) in 35 patients with prostatic carcinoma. Staging of localized tumors was based on histopathological evaluation after radial prostatectomy and pelvic lymphnode dissection (pTsub(1-3), pN0). In tumor lesions Tsub(1-2) N0 M0 elevated PAP-serum concentrations were found by RIA-determination in only one patient. Increased PAP serum levels were observed in 43-78% of carcinomas stage T3 N0 M0 and in 54-83% in stage Tsub(2-4) Nsub(x) M1 tumors, depending on the test kit used for the PAP determination. Concentrations for PAP obtained with the 4 different RIA-kits used, varied significantly and thus are not comparable. No false positive results were observed in sera of 9 patients with benign prostatic hyperplasia. Elevated PAP serum levels were found in a significantly higher frequency when determined by radioimmunoassay than by the enzymatic method. The results clearly indicate, that PAP is of no value for early recognition of carcinoma of the prostate even when measured by radioimmunoassay. However, the RIA-method seems to be of clinical importance in estimating the course of advanced local and metastasizing carcinoma of the prostate. (orig.)

  5. Method for determining microamounts of uranium in solutions from copper ores, by liquid-liquid extraction and spectrophotometry with arsenazo III.; Metodo para determinar microcantidades de uranio en disoluciones de minerales de cobre, por extraccion liquido-liquido y espectrofotometria con arsenazo III

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez, B.

    1972-07-01

    A spectrophotometric method is described for determining small amounts of uranium in aqueous solutions from copper ores. Uranium is quantitatively separated in a single extraction by a solution of tri-n-octylphosphine oxide in benzene, using ethylendiaminetetracetic acid and sodium fluoride as complexing agents, for improving the selectivity of the procedure. An aliquot of the extract is diluted with a hydrocolloidal solution of arsenazo III. Optical density is measured at 650 nm. (Author) 3 refs.

  6. [Determination of docosahexaenoic acid in milk powder by gas chromatography using acid hydrolysis].

    Science.gov (United States)

    Shao, Shiping; Xiang, Dapeng; Li, Shuang; Xi, Xinglin; Chen, Wenrui

    2015-11-01

    A method to determine docosahexenoic acid (DHA) in milk powder by gas chromatography was established. The milk powder samples were hydrolyzed with hydrochloric acid, extracted to get total fatty acids by Soxhlet extractor, then esterified with potassium hydroxide methanol solution to form methyl esters, and treated with sodium hydrogen sulfate. The optimal experiment conditions were obtained from orthogonal experiment L9(3(3)) which performed with three factors and three levels, and it requires the reaction performed with 1 mol/L potassium hydroxide solution at 25 degrees C for 5 min. The derivative treated with sodium hydrogen sulfate was separated on a column of SP-2560 (100 m x 0.25 mm x 0.20 μm), and determined in 55 min by temperature programming-gas chromatography. Good linearity was obtained in the range 5.0-300 mg/L with the correlation coefficient of 0.999 9. The relative standard deviations (RSDs) were 3.4%, 1.2% and 1.1% for the seven repeated experiments of 10, 50 and 100 mg/L of DHA, respectively. The limit of detection was 2 mg/kg, and the recoveries of DHA were in the range of 90.4%-93.5%. The results are satisfactory through the tests of practical samples. PMID:26939370

  7. Determination of free fatty acids in beer wort.

    Science.gov (United States)

    Bravi, Elisabetta; Benedetti, Paolo; Marconi, Ombretta; Perretti, Giuseppe

    2014-05-15

    The importance of free fatty acids (FFAs) in wort has been known for a long time because of their influence on beer quality and yeast metabolism. Lipids have a beneficial effect on yeast growth during fermentation as well as negative effects on beer quality. Lipids content of beer affects the ability to form a stable head of foam and plays an important role in beer staling. Moreover, the ratio of unsaturated and saturated fatty acids seems to be related to gushing problems. A novel, simple, and reliable procedure for quantitative analysis of FFAs in wort was developed and validated. The determination of FFAs in wort was achieved via liquid-liquid cartridge extraction, purification of FFA fraction by solid phase extraction, boron trifluoride in methanol methylation, and injection into GC-FID system. The proposed method has high accuracy (<0.3%, expressed as the bias), high precision (<1.2%, RSD), and recoveries ranging from 74% to 98%. The method was tested on two different wort samples (9° and 12° Plato).

  8. Determination of Fatty Acid in Asparagus by Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Zehra HAJRULAI-MUSLIU

    2016-05-01

    Full Text Available Asparagus contain a lot of macronutrients and micronutrients including folate, dietary fibre (soluble and insoluble and phenolic compounds. Also asparagus is a good source of unsaturated linoleic and linolenic fatty acids which are precursors for Eicosapentanoic acid (EPA and Docosahexanoic acid (DHA. Unsaturated fatty acids have important biological effects and they have important role in human health. The objective of this study was to analyze fatty acid composition of asparagus as a potential source of linoleic and linolenic acid - a precursor for EPA and DHA. For this reason we analyzed fifty seven samples of asparagus collected from the local market. We used AOAC 996.06 method and analyses were performed with gas chromatograph with flame-ionization detector (GC-FID. The highest concentration of fatty acid in the asparagus was linoleic acid (C18:2n6 which content in asparagus is 25.620±1.0%. Also, asparagus is good source of -linolenic fatty acid (C18:3n3 and content of this fatty acid in asparagus is 8.840±0.3%. The omega-6 to omega-3 (n6/n3 ratio in asparagus was 3.19. Polyunsaturated fatty acids (PUFAs were higher than monounsaturated fatty acids (MUFAs, and from saturated fatty acids, palmitic acid was most frequent with 24.324±1.0%. From our study we can conclude that asparagus is very good source of unsaturated fatty acids, especially linoleic and linolenic fatty acids.

  9. Qualitative and quantitative determination of naphthenic acids in Heidrun crude oil

    OpenAIRE

    2006-01-01

    ABSTRACT The main aim for the work on this thesis was to find a fast and sensitive method for qualitative and quantitative determination of the naphthenic acids (NAs) called the ARN acid family in crude oil. As there are three main components in the ARN acid family with quite similar molecular mass, separation of the acids with respect to the hydrophobicity, was essential to obtain reliable determination of all three acids. The sample preparation developed in this work consisted of liquid...

  10. Determining Phthalic Acid Esters Using Terahertz Time Domain Spectroscopy

    Science.gov (United States)

    Liu, L.; Shen, L.; Yang, F.; Han, F.; Hu, P.; Song, M.

    2016-09-01

    In this report terahertz time domain spectroscopy (THz-TDS) is applied for determining phthalic acid esters (PAEs) in standard materials. We reported the THz transmission spectrum in the frequency range of 0.2 to 2.0 THz for three PAEs: di-n-butyl phthalate (DBP), di-isononyl phthalate (DINP), and di-2-ethylhexyl phthalate ester (DEHP). The study provided the refractive indices and absorption features of these materials. The absorption spectra of three PAEs were simulated by using Gaussian software with Density Functional Theory (DFT) methods. For pure standard PAEs, the values of the refractive indices changed between 1.50 and 1.60. At 1.0 THz, the refractive indices were 1.524, 1.535, and 1.563 for DINP, DEHP, and DBP, respectively. In this experiment different concentrations of DBP were investigated using THz-TDS. Changes were measured in the low THz frequency range for refractive indices and characteristic absorption. The results indicated that THz-TDS is promising as a new method in determining PAEs in many materials. The results of this study could be used to support the practical application of THz-TDS in quality detection and food monitoring. In particular, this new technique could be used in detecting hazardous materials and other substances present in wine or foods.

  11. Flow measurement in a 170-MW hydraulic turbine using the Gibson method; Medicion del flujo de una turbina hidraulica de 170 MW utilizando el metodo Gibson

    Energy Technology Data Exchange (ETDEWEB)

    Urquiza, Gustavo [Universidad Autonoma del Estado de Morelos (Mexico); Adamkowski, Adam [The Szewalski Institute of Fluid-Flow Machinery (Poland); Kubiak, Janusz; Sierra, Fernando [Universidad Autonoma del Estado de Morelos (Mexico); Janicki, Waldemar [The Szewalski Institute of Fluid-Flow Machinery (Poland); Fernandez, J. Manuel [Comision Federal de Electricidad (Mexico)

    2007-07-15

    This paper describes the methodology applied for measuring water flow through a 170-MW hydraulic turbine. The flow rate was measured using the pressure-time method, also known as the Gibson method. This method uses the well-known water hammer phenomenon in pipelines; in turbine penstocks, for instance. The version of this method used here is based on measuring, during total stop of the water stream, the time-history of pressure change in one section of the turbine penstock and relate it to the pressure in the upper reservoir to which the penstock is connected. The volumetric flow rate is determined from the relevant integration of the measured temporary pressure rise. Flow measurement was possible this way because the influence of the penstock inlet was negligible as far as an error of the measurement is concerned. The length of the penstock was 300 m. Previous experience and a standard IEC-41-1991 were the criteria adopted and applied. A fast and efficient acquisition system, including a 16 bit card, was used. The flow rate was calculated using a computer program developed and tested on several cases. The results obtained with the Gibson method were used for calibration of the on-line flow measuring system based on the Winter-Kennedy method as one of the index methods. This method is very often used for continuous monitoring of the flow rate through hydraulic turbines, when the calibration has been done on site by using the results of measurements obtained by the absolute method. Having measured the flow rate and output power, the efficiency was calculated for any operating conditions. A curve showing the best operating conditions based on the highest efficiency is presented and discussed. The details of the instrumentation, its installation, and the results obtained are discussed in the paper. [Spanish] Este articulo describe la metodologia aplicada para la medicion del flujo en una turbina hidraulica de 170 MW. El flujo se midio utilizando el metodo de presion

  12. Determination of residues in honey after treatments with formic and oxalic acid under field conditions

    OpenAIRE

    Bogdanov, Stefan; Charrière, Jean-Daniel; IMDORF, Anton; KILCHENMANN, Verena; Fluri, Peter

    2002-01-01

    International audience Formic acid and oxalic acid field trials for control of Varroa destructor were carried out in autumn according to the Swiss prescriptions during three successive years in different apiaries in Switzerland. The following parameters were determined in honey that was harvested the year after treatment: formic acid, oxalic acid and free acidity. The following range of values were found in honeys of untreated colonies: formic acid, from 17 to 284 mg/kg, n = 34; oxalic aci...

  13. Simultaneous determination of ascorbic acid, dopamine and uric acid based on tryptophan functionalized graphene

    Energy Technology Data Exchange (ETDEWEB)

    Lian, Qianwen; He, Zhifang; He, Qian; Luo, Ai; Yan, Kaiwang; Zhang, Dongxia [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Geography and Environment Science, Northwest Normal University, Lanzhou, 730070 (China); Lu, Xiaoquan, E-mail: Luxq@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou, 730070 (China); Zhou, Xibin, E-mail: zhouxb@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Geography and Environment Science, Northwest Normal University, Lanzhou, 730070 (China)

    2014-05-01

    Highlights: • Trp-GR was synthesized by utilizing a facile ultrasonic method. • The material as prepared had well dispersivity in water and better conductivity than pure GR. • Trp-GR/GCE showed excellent potential for the determination of AA, DA and UA. • The proposed method was applied for the analysis of AA, DA and UA in real samples. - Abstract: A new type of tryptophan-functionalized graphene nanocomposite (Trp-GR) was synthesized by utilizing a facile ultrasonic method via π–π conjugate action between graphene (GR) and tryptophan (Trp) molecule. The material as prepared had well dispersivity in water and better conductivity than pure GR. The surface morphology of Trp-GR was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The electrochemical behaviors of ascorbic acid (AA), dopamine (DA), and uric acid (UA) were investigated by cyclic voltammetry (CV) on the surface of Trp-GR. The separation of the oxidation peak potentials for AA–DA, DA–UA and UA–AA was about 182 mV, 125 mV and 307 mV, which allowed simultaneously determining AA, DA, and UA. Differential pulse voltammetery (DPV) was used for the determination of AA, DA, and UA in their mixture. Under optimum conditions, the linear response ranges for the determination of AA, DA, and UA were 0.2–12.9 mM, 0.5–110 μM, and 10–1000 μM, with the detection limits (S/N = 3) of 10.09 μM, 0.29 μM and 1.24 μM, respectively. Furthermore, the modified electrode was investigated for real sample analysis.

  14. GIUSEPPE DE ROSA, Metodo per pianisti accompagnatori della danza, Milano, Suvini Zerboni, 2010

    Directory of Open Access Journals (Sweden)

    Chiara Sintoni

    2014-12-01

    Full Text Available Il volume di Giuseppe De Rosa è al contempo un agile metodo teorico-pratico per la formazione del pianista accompagnatore della danza classica e un sussidio didattico per la sua attività in situazione. Frutto dell’esperienza pluriennale dell’autore, colma un vuoto nella pubblicistica italiana dedicata all’argomento.

  15. Novel graphene flowers modified carbon fibers for simultaneous determination of ascorbic acid, dopamine and uric acid.

    Science.gov (United States)

    Du, Jiao; Yue, Ruirui; Ren, Fangfang; Yao, Zhangquan; Jiang, Fengxing; Yang, Ping; Du, Yukou

    2014-03-15

    A novel and sensitive carbon fiber electrode (CFE) modified by graphene flowers was prepared and used to simultaneously determine ascorbic acid (AA), dopamine (DA) and uric acid (UA). SEM images showed that beautiful and layer-petal graphene flowers homogeneously bloomed on the surface of CFE. Moreover, sharp and obvious oxidation peaks were found at the obtained electrode when compared with CFE and glassy carbon electrode (GCE) for the oxidation of AA, DA and UA. Also, the linear calibration plots for AA, DA and UA were observed, respectively, in the ranges of 45.4-1489.23 μM, 0.7-45.21 μM and 3.78-183.87 μM in the individual detection of each component. By simultaneously changing the concentrations of AA, DA and UA, their oxidation peaks appeared at -0.05 V, 0.16 V and 2.6 V, and the good linear responses ranges were 73.52-2305.53 μM, 1.36-125.69 μM and 3.98-371.49 μM, respectively. In addition, the obtained electrode showed satisfactory results when applied to the determination of AA, DA and UA in urine and serum samples. PMID:24140872

  16. Quantitative Determination of Citric and Ascorbic Acid in Powdered Drink Mixes

    Science.gov (United States)

    Sigmann, Samuella B.; Wheeler, Dale E.

    2004-01-01

    A procedure by which the reactions are used to quantitatively determine the amount of total acid, the amount of total ascorbic acid and the amount of citric acid in a given sample of powdered drink mix, are described. A safe, reliable and low-cost quantitative method to analyze consumer product for acid content is provided.

  17. Determination of the dissociation constants of polyepoxysuccinic acid

    Institute of Scientific and Technical Information of China (English)

    Lihua ZHANG; Zhiliang ZHU; Yanling QIU; Ronghua ZHANG; Jianfu ZHAO

    2008-01-01

    The dissociation constants of polyepoxysucci-nic acid (PESA) were investigated in this study. Based on the potentiometric titration and the BEST program, the dissociation constants of PESA were determined. Considering the complexity of the dissociation of PESA in aqueous solution, several models were constructed to simulate the dissociation process of PESA. By compar-ison, the dissociation constants of PESA were obtained with model 4. The species distribution of PESA in aque-ous solution as a function of pH was also presented according to the experimental and calculation results. It showed that the H2L model with five basic structure units to describe the dissociation of PESA was reasonable, and the relevant constants had less error and better matching between the experimental and calculation data. The cor-responding values of pKai were 4.68 and 4.92, respectively, for H2L at 35℃ with ionic strength of 0.1 mol/L.

  18. New method for the determination of bile acid turnover using /sup 75/Se-homocholic acid taurine

    Energy Technology Data Exchange (ETDEWEB)

    Delhez, H.; Meerwaldt, J.H.; van den Berg, J.W.O.; van Blankenstein, M.

    1982-06-01

    The introduction of /sup 75/Se-homocholic acid taurine (/sup 75/SeHCAT) greatly facilitates the investigation of diarrhoea of unknown origin. By using gamma-labelled bile acids, daily faecal bile acid loss can be measured in total collected stools, thus circumventing laborious mixing and sampling. The /sup 75/SeHCAT method proved to be reliable for the determination of bile acid turnover, giving results identical to the established turnover method using /sup 14/C-taurocholic acid. The new method however, is simpler and faster.

  19. Influence of educational level on determinants of folic acid use

    NARCIS (Netherlands)

    van der Pal-de Bruin, KM; de Walle, HEK; de Rover, CM; Jeeninga, W; Cornel, MC; de Jong-van den Berg, LTW; Buitendijk, SE; Paulussen, TGWM

    2003-01-01

    In The Netherlands, periconceptional folic acid use to prevent neural tube defects was promoted through a national 'Folic Acid Campaign'. In two regions, a local campaign supplemented the national campaign to increase the chances of reaching women with low socio-economic status (SES). A framework of

  20. Determination of the absolute configuration of sialic acids in gangliosides from the sea cucumber Cucumaria echinata.

    Science.gov (United States)

    Kisa, Fumiaki; Yamada, Koji; Miyamoto, Tomofumi; Inagaki, Masanori; Higuchi, Ryuichi

    2007-07-01

    Enantiomeric pairs of sialic acid, D- and L-NeuAc (N-acetylneuraminic acid), were converted to D- and L-arabinose, respectively, by chemical degradation. Using this method, the absolute configuration of the sialic acid residues, NeuAc and NeuGc (N-glycolylneuraminic acid), in the gangliosides from the sea cucumber Cucumaria echinata was determined to be the D-form. Although naturally occurring sialic acids have been believed to be the D-form on the basis of biosynthetic evidence, this is the first report of the determination of the absolute configuration of the sialic acid residues in gangliosides using chemical methods. PMID:17603199

  1. The application of hydrogen-palladium electrode for potentiometric acid-base determinations in tetrahydrofuran

    Directory of Open Access Journals (Sweden)

    Jokić Anja B.

    2013-01-01

    Full Text Available The application of the hydrogen-palladium electrode (H2/Pd as the indicator electrode for the determination of relative acidity scale (Es, mV of tetrahydrofuran (THF and the potentiometric titrations of acids in this solvent was investigated. The relative acidity scale tetrahydrofuran was determined from the difference half-neutralization potentials of perchloric acid and tetrabutylammonium hydroxide (TBAH, which were measured by using both H2/Pd-SCE and glass-SCE electrode pairs. The experimentally obtained value of Es scale THF with a H2/Pd-SCE electrode pair was 1155 mV, and those obtained with glass-SCE electrode pair 880 mV. By using a H2/Pd indicator electrode, the individual acids (benzoic acid, palmitic acid, maleic acid, acetyl acetone, α-naphthol and two component acid mixtures (benzoic acid + α-naphthol, palmitic acid + α-naphthol, maleic acid + α-naphthol and maleic acid + ftalic acid were titrated with a standard solution of TBAH. In addition, sodium methylate and potassium hydroxide proved to be very suitable titrating agents for titrating of the individual acids and the acids in mixtures, respectively. The relative error of the determination of acids in mixture was less than 3%. The results are in agreement with those obtained by a conventional glass electrode. The advantages of H2/Pd electrode over a glass electrode in potentiometric acid-base determinations in tetrahydrofuran lie in the following: this electrode gives wider relative acidity scale THF, higher the potential jumps at the titration end-point and relatively fast response time; furthermore, it is very durable, simple to prepare and can be used in the titrations of small volumes. [Projekat Ministarstva nauke Republike Srbije, br.172051

  2. Fatty acids determination in Bronte pistachios by gas chromatographic method.

    Science.gov (United States)

    Pantano, Licia; Lo Cascio, Giovanni; Alongi, Angelina; Cammilleri, Gaetano; Vella, Antonio; Macaluso, Andrea; Cicero, Nicola; Migliazzo, Aldo; Ferrantelli, Vincenzo

    2016-10-01

    A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.

  3. [Determination of arsanilic acid and sulfanilic acid as adulterant in feed additives by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Xu, Jinping; He, Heng; Xu, Mengyi; Qu, Yanhua

    2010-02-01

    A reversed-phase high performance liquid chromatographic (RP-HPLC) method was established for the determination of arsanilic acid and sulfanilic acid as adulterant in the feed additives. The separation was carried out on a Waters Bondapak C18 column, and methanol-water (pH 2.9 adjusted by 0.01 mol/L phosphoric acid) (1 : 4, v/v) was used as the mobile phase with a flow rate of 1.0 mL/min. A diode array detector was used at 244 nm as the detection wavelength. Arsanilic acid and sulfanilic acid were separated within 3 min. The linear ranges all were 5 - 200 mg/L and the detection limits (S/N = 3) were 0.20 and 0.15 mg/L for arsanilic acid and sulfanilic acid, respectively. This method is simple and rapid, and suitable for the simultaneous determination of arsanilic acid and sulfanilic acid in feed additives.

  4. Using Conductivity Measurements to Determine the Identities and Concentrations of Unknown Acids: An Inquiry Laboratory Experiment

    Science.gov (United States)

    Smith, K. Christopher; Garza, Ariana

    2015-01-01

    This paper describes a student designed experiment using titrations involving conductivity measurements to identify unknown acids as being either HCl or H[subscript 2]SO[subscript 4], and to determine the concentrations of the acids, thereby improving the utility of standard acid-base titrations. Using an inquiry context, students gain experience…

  5. DETERMINATION OF HYDROXYCINNAMIC ACIDS IN LEAVES OF PLANTAIN PLANTAGO MAJOR L. AND PLANTAGO MEDIA L.

    Directory of Open Access Journals (Sweden)

    Тая Владимировна Хортецкая

    2014-10-01

    Full Text Available By the method of thin layer chromatography is set the qualitative composition of hydroxycinnamic acids in the leaves of plantain Plantago major L. and Plantago media L. A comparative spectrophotometric determination of ortodihydrocennamic acid and chlorogenic acid amount has carried out in studied species.

  6. Influence of educational level on determinants of folic acid use.

    Science.gov (United States)

    van der Pal-de Bruin, Karin M; de Walle, Hermien E K; de Rover, Carolien M; Jeeninga, Wendy; Cornel, Martina C; de Jong-van den Berg, Lolkje T W; Buitendijk, Simone E; Paulussen, Theo G W M

    2003-07-01

    In The Netherlands, periconceptional folic acid use to prevent neural tube defects was promoted through a national 'Folic Acid Campaign'. In two regions, a local campaign supplemented the national campaign to increase the chances of reaching women with low socio-economic status (SES). A framework of outcome criteria, defined as awareness knowledge, perceived safety, attitudes and subjective norms, was developed to evaluate the effectiveness of the two local campaigns. Data were gathered by means of two cross-sectional studies conducted just before and 1 year after the campaigns took place. Before the campaigns were conducted, there were already differences in all effect criteria and folic acid use between women of different educational levels, mostly in favour of women with a high level of education. Although both educational campaigns appeared to have a positive impact on all outcome criteria, they failed to reduce the existing differences in these outcome criteria between women of different educational levels. Folic acid use can be promoted effectively by mass media campaigns, certainly in a large group of women with no prior knowledge of the health benefits associated with periconceptional folic acid use. However, in order to achieve more equal health outcomes among women of low and high SES, it seems that more tailored interventions for women of low SES are needed.

  7. Response of Substituted Indoleacetic Acids in the Indolo-alpha-pyrone Fluorescence Determination

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Böttger, M.; Kaiser, P.

    1978-01-01

    The method of indolo-.alpha.-pyrone fluorescence-determination of IAA was investigated to study possible interference from 4-chloro-indoleacetic acid and 5-hydroxyindoleacetic acid, which occur naturally. Both compounds show about 40% of the fluorescence of IAA after conversion into their .alpha.......-pyrones. Other halogenated indoleacetic acids show between zero and 60% of the fluorescence of IAA. Apparently the concentration of IAA cannot be determined in crude extracts in the presence of 4-chloro- or 5-hydroxy-indoleacetic acid, because separate determinations of each of these compounds are not possible...... by changing the excitation or fluorescence wave-lengths of the testing equipment....

  8. Determination of Enantiomeric Excess of Glutamic Acids by Lab-made Capillary Array Electrophoresis

    Institute of Scientific and Technical Information of China (English)

    Jun WANG; Kai Ying LIU; Li WANG; Ji Ling BAI

    2006-01-01

    Simulated enantiomeric excess of glutamic acid was determined by a lab-made sixteen-channel capillary array electrophoresis with confocal fluorescent rotary scanner. The experimental results indicated that the capillary array electrophoresis method can accurately determine the enantiomeric excess of glutamic acid and can be used for high-throughput screening system for combinatorial asymmetric catalysis.

  9. Probing the Specificity Determinants of Amino Acid Recognition by Arginase

    Energy Technology Data Exchange (ETDEWEB)

    Shishova, E.; Di Costanzo, L; Emig, F; Ash, D; Christianson, D

    2009-01-01

    Arginase is a binuclear manganese metalloenzyme that serves as a therapeutic target for the treatment of asthma, erectile dysfunction, and atherosclerosis. In order to better understand the molecular basis of inhibitor affinity, we have employed site-directed mutagenesis, enzyme kinetics, and X-ray crystallography to probe the molecular recognition of the amino acid moiety (i.e., the ?-amino and ?-carboxylate groups) of substrate l-arginine and inhibitors in the active site of arginase I. Specifically, we focus on (1) a water-mediated hydrogen bond between the substrate ?-carboxylate and T135, (2) a direct hydrogen bond between the substrate ?-carboxylate and N130, and (3) a direct charged hydrogen bond between the substrate ?-amino group and D183. Amino acid substitutions for T135, N130, and D183 generally compromise substrate affinity as reflected by increased KM values but have less pronounced effects on catalytic function as reflected by minimal variations of kcat. As with substrate KM values, inhibitor Kd values increase for binding to enzyme mutants and suggest that the relative contribution of intermolecular interactions to amino acid affinity in the arginase active site is water-mediated hydrogen bond < direct hydrogen bond < direct charged hydrogen bond. Structural comparisons of arginase with the related binuclear manganese metalloenzymes agmatinase and proclavaminic acid amidinohydrolase suggest that the evolution of substrate recognition in the arginase fold occurs by mutation of residues contained in specificity loops flanking the mouth of the active site (especially loops 4 and 5), thereby allowing diverse guanidinium substrates to be accommodated for catalysis.

  10. Quantitative determination of hydroxycinnamic acids in chicory root

    OpenAIRE

    Yezerska, Oksana; Kalynyuk, Tymofiy; Vronska, Lyudmula

    2013-01-01

    The possibility for applying of a direct spectrophotometry to quantify totality of hydroxycinnamic acid derivatives is investigated. As a quantitative criterion for quality assessment of chicory roots the total content of hydroxycinnamic acid derivatives of at least 0.3 %, expressed as chlorogenic acid, is suggested. Досліджено можливість застосування прямої спектрофотометрії для кількісного визначення гідроксикоричних кислот. Як кількісний критерій якості коренів цикорію запропоновано вміст...

  11. Delphinidin immobilized on silver nanoparticles for the simultaneous determination of ascorbic acid, noradrenalin, uric acid, and tryptophan

    Directory of Open Access Journals (Sweden)

    Navid Nasirizadeh

    2016-04-01

    Full Text Available In the present study, the fabrication of a new modified electrode for electrocatalytic oxidation of noradrenalin, based on the delphinidin immobilized on silver nanoparticles modified glassy carbon electrode. Cyclic voltammetry was used to investigate the redox properties of this modified electrode. The surface charge transfer rate constant (ks and the charge transfer coefficient (α for the electron transfer between the glassy carbon electrode and the immobilized delphinidin were calculated. The differential pulse voltammetry exhibited two linear dynamic ranges and a detection limit of 0.40μM for noradrenalin determination. Moreover, the present electrode could separate the oxidation peak potentials of ascorbic acid, noradrenalin, uric acid, and tryptophan in a mixture. The usefulness of this nanosensor was also investigated for the determination of ascorbic acid, noradrenalin, and uric acid in pharmaceutical and biological fluid samples with satisfactory results.

  12. DETERMINATION OF CARBOXYLIC ACIDS BY ION-EXCLUSION CHROMATOGRAPHY WITH NON-SUPPRESSED CONDUCTIVITY AND OPTICAL DETECTORS

    Science.gov (United States)

    Determination of carboxylic acids using non-suppressed conductivity and UV detections is described. The background conductance of 1-octanesulfonic acid, hexane sulfonic acid and sulfuric acid at varying concentrations was determined. Using 0.2 mM 1-octanesulfonic acid as a mobile...

  13. Ion-exclusion chromatography determination of organic acid in uridine 5'-monophosphate fermentation broth.

    Science.gov (United States)

    Niu, Huanqing; Chen, Yong; Xie, Jingjing; Chen, Xiaochun; Bai, Jianxin; Wu, Jinglan; Liu, Dong; Ying, Hanjie

    2012-09-01

    Simultaneous determination of organic acids using ion-exclusion liquid chromatography and ultraviolet detection is described. The chromatographic conditions are optimized when an Aminex HPX-87H column (300 × 7.8 mm) is employed, with a solution of 3 mmol/L sulfuric acid as eluent, a flow rate of 0.4 mL/min and a column temperature of 60°C. Eight organic acids (including orotic acid, α-ketoglutaric acid, citric acid, pyruvic acid, malic acid, succinic acid, lactic acid and acetic acid) and one nucleotide are successfully quantified. The calibration curves for these analytes are linear, with correlation coefficients exceeding 0.999. The average recovery of organic acids is in the range of 97.6% ∼ 103.1%, and the relative standard deviation is in the range of 0.037% ∼ 0.38%. The method is subsequently applied to obtain organic acid profiles of uridine 5'-monophosphate culture broth fermented from orotic acid by Saccharomyces cerevisiae. These data demonstrate the quantitative accuracy for nucleotide fermentation mixtures, and suggest that the method may also be applicable to other biological samples. PMID:22634191

  14. Occurrence and Determination of Haloacetic Acids in Metro Manila Drinking Water

    Directory of Open Access Journals (Sweden)

    Irene B. Rodriguez

    2009-12-01

    Full Text Available Haloacetic acids are found in chlorinated water with high organic matter content. An analytical method based on a US EPA method for measuring these compounds in water is described. The optimized method used diethyl ether as extraction solvent with sulphuric acid-methanol as esterification agent and subsequent detection by gas chromatography-electron capture detection. Evaluation of this method showed that it was linear in the concentration range of 10 to 150 µg L-1 and the method detection limits were from 17 to 57 µg L-1. Although the method demonstrated low recoveries (16 to 43%, it is useful in the quantitative determination of monochloroacetic acid as well as the qualitative determination of other haloacetic acids in water. Drinking water samples taken from different areas in Metro Manila serviced by the local treatment plants were analysed using the method. Monochloroacetic acid, monobromoacetic acid, and bromochloroacetic acid were detected in these samples. Monochloroacetic acid was quantified and found in concentrations ranging from 19 to 157 µg L-1. In most of the water samples, the concentration of monochloroacetic acid exceeded the US EPA maximum allowable total concentration of 60 µg L-1 for the five haloacetic acids (monochloro-, dichloro-, trichloro-, monobromo-, and dibromoacetic acids in drinking water. This initial study established the occurrence of potentially harmful haloacetic acids in the local drinking water supplies.

  15. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Maurya, Anupam; Srivastava, Santosh Kumar [Analytical Chemistry Division, Central Institute of Medicinal and Aromatic Plants, Lucknow (India)

    2012-03-15

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 {sup m}u{sup m}) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL{sup -1} (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 {mu}g for ursolic acid, and 0.176 and 0.587 {mu}g for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  16. Amino Acid Profile as a Feasible Tool for Determination of the Authenticity of Fruit Juices

    OpenAIRE

    Mostafa Asadpoor; Masoud Ansarin; Mahboob Nemati

    2014-01-01

    Purpose: Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. Methods: The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA). Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the...

  17. Determination of Total Acid in Palygorskite Chemically Modified by N-Butylamine Thermodesorption

    Directory of Open Access Journals (Sweden)

    Ruiz Juan A.C.

    2002-01-01

    Full Text Available The acid properties of palygorskite clay (R1 were studied using n-butylamine as probe molecule. A comparison was made of these properties in palygorskite clay (R1, in an acidified palygorskite (R2 and in acid palygorskite loaded with 2% of lanthanum (R3. The total acid properties were determined by FTIR (Fourier Transform Infrared and TG-DTA (thermogravimetry. The acidity increased as follows: R3>R2>R1. The acid strength sites were classified as physisorbed, weak, medium and strong. The acid treatment did not change the site distribution, apparently only removing channel impurities. The introduction of lanthanum created many more acid sites and increased the specific area. Both weak and strong sites, which increased significantly, were considered new active acid sites produced by the lanthanum.

  18. Determination of nitrite ion and sulfanilic and orthanilic acids by differential pulse polarography

    Energy Technology Data Exchange (ETDEWEB)

    Sulaiman, S.T.

    1984-11-01

    The nitrite ion can be determined with a high degree of accuracy and sensitivity by differential pulse polarography utilizing the rapid and quantitative reaction between the nitrite ion and sulfanilic acid or orthanilic acid at pH 1.5. The experimental detection limit is shown to be 8.6 X 10/sup -8/ M (as NO/sub 2//sup -/) in simple aqueous solution. The method is further used to determine concentrations of sulfanilic acid down to 4 X 10/sup -7/ M and orthanilic acid down to 1.6 X 10/sup -6/ M under optimum conditions.

  19. Quality control of herbs: determination of amino acids in Althaea officinalis, Matricaria chamomilla and Taraxacum officinale.

    Science.gov (United States)

    Qureshi, Muhammad Nasimullah; Stecher, Guenther; Bonn, Guenther Karl

    2014-05-01

    Analysis of raw materials and final products need reliable methods for the standardization of natural product drugs. Legal guideline also emphasizes on the qualitative and quantitative analyses of the plant constituents in an herbal product. In this study, thin layer chromatography (TLC) and amino acid analyzer was used for the determination of amino acids in plant extracts. Samples for this study were standards and aqueous extracts from Althaea officinalis, Matricaria chamomilla and Taraxacum officinale. Different amino acids in the extracts were detected through TLC. An automatic amino acid analyzer was used for the quantification of amino acids in the plant extracts under study. PMID:24811801

  20. Determination of phenolic acids in olive oil by capillary electrophoresis.

    Science.gov (United States)

    Buiarelli, Francesca; Di Berardino, Sonia; Coccioli, Franco; Jasionowska, Renata; Russo, Mario Vincenzo

    2004-01-01

    A CZE method for the separation and quantitation of phenolic acids (cinnamic, syringic, p-coumaric, vanillic, caffeic, 3,4-dihydroxyphenylacetic, protocatechuic), extracted from extra virgin olive oil, was developed. The sample preparation involved the LLE and SPE extraction methods. CE separation was performed in a fused silica capillary of I.D.= 50microm using as a BGE 40 mM borate buffer at pH=9.2. The separation voltage was 18kV with corresponding current of 27-28 microA. Detection was accomplished with UV-detector at lambda=200nm. The proposed method was fully validated. A good repeatability of migration time (RSD% ranged from 0.81 to 1.63) and of corrected peak area (RSD% from 2.89 to 5.77) was obtained. The linearity of detector response in the range from 5 to 50 ppm was checked, obtaining the correlation coefficient R2 values in the range: 0.9919-0.9997. Some phenolic acids in real oil samples were detected and quantified with the proposed method. PMID:15506620

  1. Spectrofluorimetric determination of gallium with calon-carboxylic acid

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A simple and sensitive spectrofluorimetric procedure for the analysis of microquantities of gallium in alloy wasdescribed. The method is based on the formation of Ga(Ⅲ)-CCA (calon-carboxylic acid) complex. The emission of thefluorescent complex was measured at λ = 620 nm with excitation at λ = 584 nm. A good linearity was found in the galliumrange of 0.7-280 ng/mL. The precision of the method is good and the relative standard deviation is 1.9% for a gallium stan-dard solution of 70 ng/mL. The procedure was proved to be suitable in terms of accuracy and selectivity for the mi-croamount of gallium in alloy.

  2. SIMULTANEOUS DETERMINATION OF CHLORINE DIOXIDE AND HYPOCHLOROUS ACID IN BLEACHING SYSTEM

    Directory of Open Access Journals (Sweden)

    Qiang Wang

    2011-04-01

    Full Text Available This study has demonstrated a rapid spectroscopic method for the determination of chlorine dioxide and hypochlorous acid concentrations in the pulp bleaching processes. It was found that chlorine dioxide and hypochlorous acid have an isosbestic wavelength of 295 nm. The soluble lignin in such a system is the main interference, but can be corrected by determining the absorbances at 295 nm, 380 nm, and 480 nm. Thus, based on the spectroscopic measurements at 295 nm (the isosbestic point wavelength for chlorine dioxide and hypochlorous acid, 380 nm (absorbance wavelength of chlorine dioxide and 480 nm (the acid soluble lignin absorbance wavelength, the chlorine dioxide and hypochlorous acid concentrations in the bleaching process can be quantified. However, hypochlorous acid was not detected in the real bleaching effluent for its low content. The present method is simple, rapid, accurate, and has the potential for on-line monitoring of the chlorine dioxide bleaching process.

  3. Determination of Five Organic Acids in Radix Isatidis by Column Partition Chromatography and Capillary Zone Electrophoresis

    Institute of Scientific and Technical Information of China (English)

    CHAIYi-fen; JISong-gang; ZHANGGuo-qing; LIUChang-hai

    2003-01-01

    Aim To determine five organic acids in Radix lsatidis. Method The extraction method and the column partition chromatographic conditiom were studied. Then a capillary zone dectrophorefic method was set up for the determina-tion. Results The linear ranges of quinazolinone acid, n-anthranilic acid, benzoic acid, salicylic acid, and syringic acid were 5.52 - 92.0μg·mL-1 , 5.12 - 102μg·mL-1 , 2.28 - 84.4μg·mL-1, 4.78 - 159 μg·mL-1, and 1.74- 87.0μg·mL-1 respectively. Conclusion The established method is accurate and simple.

  4. Determination of free and total phenolic acids in plant-derived foods by HPLC with diode-array detection.

    Science.gov (United States)

    Mattila, Pirjo; Kumpulainen, Jorma

    2002-06-19

    A high-performance liquid chromatographic (HPLC) method with diode-array detection (DAD) was used to identify and quantify free and total phenolic acids (m-hydroxybenzoic acid, p-hydroxybenzoic acid, protocatechuic acid, gallic acid, vanillic acid, syringic acid, o-coumaric acid, m-coumaric acid, p-coumaric acid, caffeic acid, ferulic acid, sinapic acid, chlorogenic acid, and ellagic acid) in plant foods. Free phenolic acids were extracted with a mixture of methanol and 10% acetic acid. Bound phenolic acids were liberated using first alkaline and then acid hydrolysis followed by extraction with diethyl ether/ethyl acetate (1:1). All fractions were quantified separately by HPLC. After HPLC quantification, results of alkali and acid hydrolysates were calculated to represent total phenolic acids. Ellagic acid was quantified separately after long (20 h) acid hydrolysis. The methods developed were effective for the determination of phenolic acids in plant foods. DAD response was linear for all phenolic acids within the ranges evaluated, with correlation coefficients exceeding 0.999. Coefficients of variation for 4-8 sample replicates were consistently below 10%. Recovery tests of phenolic acids were performed for every hydrolysis condition using several samples. Recoveries were generally good (mean >90%) with the exceptions of gallic acid and, in some cases, caffeic acid samples. PMID:12059140

  5. [Gas chromatographic determination of formic acid in urine as carbon monoxide (author's transl)].

    Science.gov (United States)

    Angerer, J

    1976-02-01

    A gas chromatographic method for determining formic acid in human urine is described. The analytical reliability of this method fullfills the criteria of statistical quality control. The rate of recovery is 101.2 to 105.7% the variability coefficients lie between 2.9 and 7.2%. The selectivity of this method is demonstrated by analysing a group of components normally occuring in urine which did not interfere with the determination of formic acid. The detection limit of about 4.3 mumol/1 formic acid in urine permits the determination of the concentration of formic acid in the urine of normal persons. The concentrations of formic acid in the urine of a group of normal persons lies between 0 and 2.79 mmol/1. The average concentration was 0.39 +/- 0.60 mmol/1. PMID:1249528

  6. Uronic acid determination by high performance liquid chromatography with postcolumn fluorescence derivatization.

    Science.gov (United States)

    Kakita, Hirotaka; Kamishima, Hiroshi; Inouye, Kuniyo

    2006-10-01

    To develop a fluorimetric high performance liquid chromatography (HPLC) technique for uronic acid microanalysis, a saline mobile phase and the postcolumn fluorimetric determination were combined. The detection limits of D-glucuronic, D-galacturonic and D-mannuronic acids were 7.19, 23.88 and 7.08 pmol, respectively. The proposed method was successfully applied to uronic acid microanalysis in a polysaccharide hydrolysate and a drink. PMID:16956616

  7. Determinants of cyanuric acid and melamine assembly in water.

    Science.gov (United States)

    Ma, Mingming; Bong, Dennis

    2011-07-19

    While the recognition of cyanuric acid (CA) by melamine (M) and their derivatives has been known to occur in both water and organic solvents for some time, analysis of CA/M assembly in water has not been reported (Ranganathan, A.; Pedireddi, V. R.; Rao, C. N. R. J. Am. Chem. Soc.1999, 121, 1752-1753; Mathias, J. P.; Simanek, E. E.; Seto, C. T.; Whitesides, G. M. Macromol. Symp.1994, 77, 157-166; Zerkowski, J. A.; MacDonald, J. C.; Seto, C. T.; Wierda, D. A.; Whitesides, G. M. J. Am. Chem. Soc.1994, 116, 2382-2391; Mathias, J. P.; Seto, C. T.; Whitesides, G. M. Polym. Prepr.1993, 34, 92-93; Seto, C. T.; Whitesides, G. M. J. Am. Chem. Soc.1993, 115, 905-916; Zerkowski, J. A.; Seto, C. T.; Whitesides, G. M. J. Am. Chem. Soc.1992, 114, 5473-5475; Seto, C. T.; Whitesides, G. M. J. Am. Chem. Soc.1990, 112, 6409-6411; Wang, Y.; Wei, B.; Wang, Q. J. Chem. Cryst.1990, 20, 79-84; ten Cate, M. G. J.; Huskens, J.; Crego-Calama, M.; Reinhoudt, D. N. Chem.-Eur. J.2004, 10, 3632-3639). We have examined assembly of CA/M, as well as assembly of soluble trivalent CA and M derivatives (TCA/TM), in aqueous solvent, using a combination of solution phase NMR, isothermal titration and differential scanning calorimetry (ITC/DSC), cryo-transmission electron microscopy (cryo-TEM), and synthetic chemistry. While the parent heterocycles coprecipitate in water, the trivalent system displays more controlled and cooperative assembly that occurs at lower concentrations than the parent and yields a stable nanoparticle suspension. The assembly of both parent and trivalent systems is rigorously 1:1 and proceeds as an exothermic, proton-transfer coupled process in neutral pH water. Though CA and M are considered canonical hydrogen-bonding motifs in organic solvents, we find that their assembly in water is driven in large part by enthalpically favorable surface-area burial, similar to what is observed with nucleic acid recognition. There are currently few synthetic systems capable of robust molecular

  8. Development of an Analytical System for Determination of Free Acid via a Joint Method Combining Density and Conductivity Measurement

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    Determination of free acid plays an important role in spent nuclear fuel reprocessing. It is necessary to develop a rapid analytical device and method for measuring free acid. A novel analytical system and method was studied to monitor the acidity

  9. Simultaneous determination of free amino acids in Pu-erh tea and their changes during fermentation.

    Science.gov (United States)

    Zhu, Yuchen; Luo, Yinghua; Wang, Pengpu; Zhao, Mengyao; Li, Lei; Hu, Xiaosong; Chen, Fang

    2016-03-01

    Pu-erh ripened tea is produced through a unique microbial fermentation process from the sun-dried leaves of large-leaf tea species (Camellia sinensis (Linn.) var. assamica (Masters) Kitamura) in Yunnan province of China. In this study, the changes of amino acid profiles during fermentation of Pu-erh tea were investigated, based on the improved HPLC-UV method with PITC pre-column derivatization for the simultaneous determination of twenty free amino acids. Results showed that aspartic acid, glutamic acid, arginine, alanine, theanine and tyrosine were the major amino acids in tea samples. Fermentation significantly influenced on the amino acid profiles. The total free amino acid contents significantly decreased during fermentation (ptea.

  10. [Determination of body fluid based on analysis of nucleic acids].

    Science.gov (United States)

    Korabečná, Marie

    2015-01-01

    Recent methodological approaches of molecular genetics allow isolation of nucleic acids (DNA and RNA) from negligible forensic samples. Analysis of these molecules may be used not only for individual identification based on DNA profiling but also for the detection of origin of the body fluid which (alone or in mixture with other body fluids) forms the examined biological trace. Such an examination can contribute to the evaluation of procedural, technical and tactical value of the trace. Molecular genetic approaches discussed in the review offer new possibilities in comparison with traditional spectrum of chemical, immunological and spectroscopic tests especially with regard to the interpretation of mixtures of biological fluids and to the confirmatory character of the tests. Approaches based on reverse transcription of tissue specific mRNA and their subsequent polymerase chain reaction (PCR) and fragmentation analysis are applicable on samples containing minimal amounts of biological material. Methods for body fluid discrimination based on examination of microRNA in samples provided so far confusing results therefore further development in this field is needed. The examination of tissue specific methylation of nucleotides in selected gene sequences seems to represent a promising enrichment of the methodological spectrum. The detection of DNA sequences of tissue related bacteria has been established and it provides satisfactory results mainly in combination with above mentioned methodological approaches. PMID:26419517

  11. Electrocatalytic and simultaneous determination of isoproterenol, uric acid and folic acid at molybdenum (VI) complex-carbon nanotube paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Beitollahi, Hadi, E-mail: h.beitollahi@yahoo.com [Environment Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Sheikhshoaie, Iran [Department of Chemistry, Faculty of Science, Shahid Bahonar University of Kerman, Kerman 76175-133 (Iran, Islamic Republic of)

    2011-11-30

    Highlights: > A molybdenum (VI) complex-carbon nanotube paste electrode have been fabricated. > This electrode reduced the oxidation potential of isoproterenol by about 175 mV. > It resolved the voltammetric waves of isoproterenol, uric acid and folic acid. - Abstract: This paper describes the development, electrochemical characterization and utilization of a novel modified molybdenum (VI) complex-carbon nanotube paste electrode for the electrocatalytic determination of isoproterenol (IP). The electrochemical profile of the proposed modified electrode was analyzed by cyclic voltammetry (CV) that showed a shift of the oxidation peak potential of IP at 175 mV to less positive value, compared with an unmodified carbon paste electrode. Differential pulse voltammetry (DPV) in 0.1 M phosphate buffer solution (PBS) at pH 7.0 was performed to determine IP in the range from 0.7 to 600.0 {mu}M, with a detection limit of 35.0 nM. Then the modified electrode was used to determine IP in an excess of uric acid (UA) and folic acid (FA) by DPV. Finally, this method was used for the determination of IP in some real samples.

  12. Determination of trans fatty acid levels by FTIR in processed foods in Australia.

    Science.gov (United States)

    McCarthy, Justine; Barr, Daniel; Sinclair, Andrew

    2008-01-01

    Health authorities around the world advise 'limiting consumption of trans fatty acid', however in Australia the trans fatty acid (TFA) content is not required to be listed in the nutrition information panel unless a declaration or nutrient claim is made about fatty acids or cholesterol. Since there is limited knowledge about trans fatty acid levels in processed foods available in Australia, this study aimed to determine the levels of TFA in selected food items known to be sources of TFA from previously published studies. Food items (n=92) that contain vegetable oil and a total fat content greater than 5% were included. This criterion was used in conjunction with a review of similar studies where food items were found to contain high levels of trans fatty acids. Lipids were extracted using solvents. Gravimetric methods were used to determine total fat content and trans fatty acid levels were quantified by Attenuated Total Reflectance Fourier Transform Infrared spectroscopy. High levels of trans fatty acids were found in certain items in the Australian food supply, with a high degree of variability. Of the samples analysed, 13 contained greater than 1 g of trans fatty acids per serving size, the highest value was 8.1 g/serving. Apart from when the nutrition information panel states that the content is less than a designated low level, food labels sold in Australia do not indicate trans fatty acid levels. We suggested that health authorities seek ways to assist consumers to limit their intakes of trans fatty acids. PMID:18818158

  13. An automatic system for acidity determination based on sequential injection titration and the monosegmented flow approach.

    Science.gov (United States)

    Kozak, Joanna; Wójtowicz, Marzena; Gawenda, Nadzieja; Kościelniak, Paweł

    2011-06-15

    An automatic sequential injection system, combining monosegmented flow analysis, sequential injection analysis and sequential injection titration is proposed for acidity determination. The system enables controllable sample dilution and generation of standards of required concentration in a monosegmented sequential injection manner, sequential injection titration of the prepared solutions, data collecting, and handling. It has been tested on spectrophotometric determination of acetic, citric and phosphoric acids with sodium hydroxide used as a titrant and phenolphthalein or thymolphthalein (in the case of phosphoric acid determination) as indicators. Accuracy better than |4.4|% (RE) and repeatability better than 2.9% (RSD) have been obtained. It has been applied to the determination of total acidity in vinegars and various soft drinks. The system provides low sample (less than 0.3 mL) consumption. On average, analysis of a sample takes several minutes. PMID:21641455

  14. Ascorbic Acid Determination in Natural Orange Juice: As a Teaching Tool of Coulometry and Polarography.

    Science.gov (United States)

    Bertotti, Mauro; And Others

    1995-01-01

    Describes an experiment designed to determine ascorbic acid concentrations in natural orange juice. The experiment is used with undergraduate pharmacy students to allow understanding of the principles of operation of the coulometer and polarograph. (DDR)

  15. A Simple Spectrophotometric Method for the Determination of Thiobarbituric Acid Reactive Substances in Fried Fast Foods.

    Science.gov (United States)

    Zeb, Alam; Ullah, Fareed

    2016-01-01

    A simple and highly sensitive spectrophotometric method was developed for the determination of thiobarbituric acid reactive substances (TBARS) as a marker for lipid peroxidation in fried fast foods. The method uses the reaction of malondialdehyde (MDA) and TBA in the glacial acetic acid medium. The method was precise, sensitive, and highly reproducible for quantitative determination of TBARS. The precision of extractions and analytical procedure was very high as compared to the reported methods. The method was used to determine the TBARS contents in the fried fast foods such as Shami kebab, samosa, fried bread, and potato chips. Shami kebab, samosa, and potato chips have higher amount of TBARS in glacial acetic acid-water extraction system than their corresponding pure glacial acetic acid and vice versa in fried bread samples. The method can successfully be used for the determination of TBARS in other food matrices, especially in quality control of food industries. PMID:27123360

  16. A Simple Spectrophotometric Method for the Determination of Thiobarbituric Acid Reactive Substances in Fried Fast Foods

    Directory of Open Access Journals (Sweden)

    Alam Zeb

    2016-01-01

    Full Text Available A simple and highly sensitive spectrophotometric method was developed for the determination of thiobarbituric acid reactive substances (TBARS as a marker for lipid peroxidation in fried fast foods. The method uses the reaction of malondialdehyde (MDA and TBA in the glacial acetic acid medium. The method was precise, sensitive, and highly reproducible for quantitative determination of TBARS. The precision of extractions and analytical procedure was very high as compared to the reported methods. The method was used to determine the TBARS contents in the fried fast foods such as Shami kebab, samosa, fried bread, and potato chips. Shami kebab, samosa, and potato chips have higher amount of TBARS in glacial acetic acid-water extraction system than their corresponding pure glacial acetic acid and vice versa in fried bread samples. The method can successfully be used for the determination of TBARS in other food matrices, especially in quality control of food industries.

  17. Rapid simultaneous determination of organic acids, free amino acids, and lactose in cheese by capillary electrophoresis.

    Science.gov (United States)

    Izco, J M; Tormo, M; Jiménez-Flores, R

    2002-09-01

    A capillary electrophoresis (CE) method for the simultaneous separation of 11 metabolically important organic acids (oxalic, formic, citric, succinic, orotic, uric, acetic, pyruvic, propionic, lactic, and butyric), 10 amino acids (Asp, Glu, Tyr, Gly, Ala, Ser, Leu, Phe, Lys, and Trp), and lactose has been optimized, validated, and tested in dairy products. Repeatability and linearity were calculated for each compound, with detection limit values as low as 0.2 x 10(-2) mM for citric acid and Gly. The method was applied to analyze yogurt and different varieties of commercial cheeses. This method yielded specific CE patterns for different varieties of cheese. Also, it has been shown to be sensitive enough to measure small changes in composition of some of those compounds in fresh cheese stored under accelerated ripening conditions for 2 d at 32 degrees C (e.g., from 1728.3 +/- 45.0 to 1166.7 +/- 4.5 mg/100 g of DM in the case of lactose, or from 23.5 +/- 0.6 to 76.8 +/- 16.7 mg/100 g of DM in the case of acetic acid).

  18. Determining important regulatory relations of amino acids from dynamic network analysis of plasma amino acids.

    Science.gov (United States)

    Shikata, Nahoko; Maki, Yukihiro; Nakatsui, Masahiko; Mori, Masato; Noguchi, Yasushi; Yoshida, Shintaro; Takahashi, Michio; Kondo, Nobuo; Okamoto, Masahiro

    2010-01-01

    The changes in the concentrations of plasma amino acids do not always follow the flow-based metabolic pathway network. We have previously shown that there is a control-based network structure among plasma amino acids besides the metabolic pathway map. Based on this network structure, in this study, we performed dynamic analysis using time-course data of the plasma samples of rats fed single essential amino acid deficient diet. Using S-system model (conceptual mathematical model represented by power-law formalism), we inferred the dynamic network structure which reproduces the actual time-courses within the error allowance of 13.17%. By performing sensitivity analysis, three of the most dominant relations in this network were selected; the control paths from leucine to valine, from methionine to threonine, and from leucine to isoleucine. This result is in good agreement with the biological knowledge regarding branched-chain amino acids, and suggests the biological importance of the effect from methionine to threonine.

  19. Fast online determination of surfactant inhibition in acidic phase bioreactors.

    Science.gov (United States)

    Feitkenhauer, H

    2004-01-01

    Surfactants have been shown to inhibit the anaerobic digestion process severely, with the methanogenic microorganisms being the most affected. The diverse nature of surfactants used even in one (e.g. textile finishing) plant makes an online determination of surfactants sometimes very difficult and expensive. Therefore a fast online determination of inhibitory effects on the acidogenic microorganisms (first step of the degradation cascade) can help to give an early warning signal or to calculate a "pseudo"-surfactant concentration. In a two-phase system this information can be used to protect the methanogenic reactor against surfactant overloading and its long term negative effects. In this paper it is shown that the inhibition is a consequence of microbial inhibition and is not caused by an inactivation of extracellular hydrolytic enzymes (released by the cells for biopolymer cleavage). A titration technique was successfully employed to measure the surfactant inhibition in a laboratory-scale acidification reactor. Additional experiments demonstrate (using sodium dodecyl sulfate as the model substance) how inhibitory effects (and strategies to overcome inhibitory effects) can be investigated efficiently. PMID:14979534

  20. SIMULTANEOUS DETERMINATION OF CHLORINE DIOXIDE AND HYPOCHLOROUS ACID IN BLEACHING SYSTEM

    OpenAIRE

    Qiang Wang; Kefu Chen; Jun Li Mail; Jun Xu; Shanshan Liu Mail

    2011-01-01

    This study has demonstrated a rapid spectroscopic method for the determination of chlorine dioxide and hypochlorous acid concentrations in the pulp bleaching processes. It was found that chlorine dioxide and hypochlorous acid have an isosbestic wavelength of 295 nm. The soluble lignin in such a system is the main interference, but can be corrected by determining the absorbances at 295 nm, 380 nm, and 480 nm. Thus, based on the spectroscopic measurements at 295 nm (the isosbestic point wavelen...

  1. A Simple Spectrophotometric Method for the Determination of Thiobarbituric Acid Reactive Substances in Fried Fast Foods

    OpenAIRE

    Alam Zeb; Fareed Ullah

    2016-01-01

    A simple and highly sensitive spectrophotometric method was developed for the determination of thiobarbituric acid reactive substances (TBARS) as a marker for lipid peroxidation in fried fast foods. The method uses the reaction of malondialdehyde (MDA) and TBA in the glacial acetic acid medium. The method was precise, sensitive, and highly reproducible for quantitative determination of TBARS. The precision of extractions and analytical procedure was very high as compared to the reported metho...

  2. Site specific incorporation of heavy atom-containing unnatural amino acids into proteins for structure determination

    Science.gov (United States)

    Xie, Jianming; Wang, Lei; Wu, Ning; Schultz, Peter G.

    2008-07-15

    Translation systems and other compositions including orthogonal aminoacyl tRNA-synthetases that preferentially charge an orthogonal tRNA with an iodinated or brominated amino acid are provided. Nucleic acids encoding such synthetases are also described, as are methods and kits for producing proteins including heavy atom-containing amino acids, e.g., brominated or iodinated amino acids. Methods of determining the structure of a protein, e.g., a protein into which a heavy atom has been site-specifically incorporated through use of an orthogonal tRNA/aminoacyl tRNA-synthetase pair, are also described.

  3. Determination of silica in silicates by differential spectrophotometry as α-molybdosilicic acid

    International Nuclear Information System (INIS)

    A method for determining silica in silicates by differential spectrophotometry, using β-molybdosilic acid, is described. The sample is attacked by a mixture of boron trioxide and lithium carbonate (10:1). α-molydbosilicic acid is developed in a buffered solution (pH approximatelly 3.9) containing acetic acid and sodium acetate. The analytical procedure involves a series of preliminary steps which were previously elaborated for the gravimetric determination of silica as oxine molybdosilicate and which account for the removal of phosphorus, titanium and zirconium through ion exchange resins. (C.L.B.)

  4. Voltammetric determination of salicylic acid in pharmaceuticals formulations of acetylsalicylic acid.

    Science.gov (United States)

    Torriero, Angel A J; Luco, Juan M; Sereno, Leonides; Raba, Julio

    2004-02-01

    The electrochemical oxidation of salicylic acid (SA) has been studied on a glassy carbon electrode using cyclic voltammetry and differential pulse voltammetric (DPV) method. SA gives a single irreversible oxidation wave over the wide pH range studied. The irreversibility of the electrode process was verified by different criteria. The mechanism of oxidation is discussed. Using differential pulse voltammetry, SA yielded a well-defined voltammetric response in Britton-Robinson buffer solution, pH 2.37 at 1.088V (versus Ag/AgCl). The method was linear over the SA concentration range: 1-60mugml(-1). The method was successfully applied for the analysis of SA as a hydrolysis product, in solid pharmaceutical formulations containing acetylsalicylic acid (ASA). PMID:18969288

  5. Chemiluminescence determination of folic acid by a flow injection analysis assembly

    Science.gov (United States)

    Wabaidur, Saikh Mohammad; Alam, Seikh Mafiz; Lee, Sang Hak; Alothman, Zeid Abdullah; Eldesoky, Gaber E.

    2013-03-01

    A flow injection (FI) method is reported for the determination of folic acid by chemiluminescence method. This method is based on the reaction of folic acid with Ru(bipy)32+ and Ce(IV) to produce chemiluminescence. The calibration curve was linear over the range of 2.5 × 10-5-3.1 × 10-7 mol/L with a detection limit of 2.3 × 10-8 mol/L (S/N = 3). The relative standard deviation of 1.0 × 10-6 mol/L folic acid was found 3.5% (n = 11). The influences of potential interfering substances were studied. The recovery was higher than 95.3%. The method was accurate, sensitive, and effective for assay of folic acid. This CL method was successfully applied to the determination of folic acid in pharmaceutical preparations. The mechanism of CL reaction was also studied.

  6. Determination of cinnamic acid in human urine by flow injection chemiluminescence

    Directory of Open Access Journals (Sweden)

    Xuemei Fan

    2011-01-01

    Full Text Available It was found that cinnamic acid can react with potassium permanganate in the acidic medium and produce chemiluminescence, which was greatly enhanced by glyoxal. Under the optimum conditions, the linear range for the determination of cinnamic acid was 1.0×10-8 to 1.0×10-4 mol L-1 with a detection limit of 8.0×10-9 mol L-1, the relative standard deviation was 1.7% for 2.0×10-6 mol L-1 cinnamic acid solution in nine repeated measurements. This method was found to be novel0simple0fast and sensitive, it was successfully applied to the determination of cinnamic acid in human urine. Furthermore, the possible reaction mechanism was also discussed.

  7. Fluorimetric determination of total ascorbic acid by a stopped-flow mixing technique.

    Science.gov (United States)

    Pérez-Ruiz, T; Martínez-Lozano, C; Tomás, V; Fenoll, J; Fenol, J

    2001-08-01

    A simple, rapid and automatic fluorimetric method for the determination of total ascorbic acid is described. The method makes use of the stopped-flow mixing technique in order to achieve the rapid oxidation of ascorbic acid by dissolved oxygen to dehydroascorbic acid, which then reacts with o-phenylenediamine to form a fluorescent quinoxaline. The initial rate and fluorescence signal of this system are directly proportional to the ascorbic acid concentration. The calibration graph was linear over the range 0.1-30 microg ml(-1) (kinetic method) and 0.25-34 microg ml(-1) (equilibrium method). The precision (% RSD) was close to 0.5%. The method has been used for the determination of ascorbic acid in pharmaceutical formulations, fruit juices, soft drinks and blood serum. PMID:11534621

  8. Determination of fatty acid composition of γ-irradiated hazelnuts, walnuts, almonds, and pistachios

    Science.gov (United States)

    Gecgel, Umit; Gumus, Tuncay; Tasan, Murat; Daglioglu, Orhan; Arici, Muhammet

    2011-04-01

    Hazelnut, walnut, almonds, and pistachio nuts were treated with 1, 3, 5, and 7 kGy of gamma irradiation, respectively. Oil content, free fatty acid, peroxide value, and fatty acid composition of the nuts were investigated immediately after irradiation. The data obtained from the experiments indicated that gamma irradiation did not cause any significant change in the oil content of nuts. In contrast, free fatty acid and peroxide value of the nuts increased proportionally to the dose (p<0.05). Among the fatty acids determined, the concentration of total saturated fatty acids increased while total monounsaturated and total polyunsaturated fatty acids decreased with the irradiation dose (p<0.05 and <0.01).

  9. Rapid determination of dipicolinic acid in the spores of Clostridium species by gas-liquid chromatography.

    Science.gov (United States)

    Tabor, M W; MacGee, J; Holland, J W

    1976-01-01

    A gas-liquid chromatographic procedure has been developed to quantitate dipicolinic acid in bacterial spores. The culture, washed from a plate, was hydrolyzed with acid containing the internal standard, pyridine-2,4-dicarboxylate, and then extracted into methyl isobutyl ketone. The internal standard and dipicolinic acid were then extracted into a small volume of trimethylphenylammonium hydroxide. Injection of the resultant quaternary ammonium salts into a gas chromatograph yielded, via thermal decomposition, the methyl ester derivatives of the dipicolinic acid and the internal standard. The amount of dipicolinic acid in the sample was determined from a standard curve. The method was sensitive to 100 ng of dipicolinic acid per sample and was 1,000 to 5,000 times more sensitive than the commonly used methods. Preparation of the sample required less than 1.5 h and less than 15 min of the analyst's time. PMID:942206

  10. Determination of fatty acid composition of {gamma}-irradiated hazelnuts, walnuts, almonds, and pistachios

    Energy Technology Data Exchange (ETDEWEB)

    Gecgel, Umit, E-mail: ugecgel@nku.edu.t [Namik Kemal University, Agricultural Faculty, Department of Food Engineering, 59030 Tekirdag (Turkey); Gumus, Tuncay; Tasan, Murat; Daglioglu, Orhan; Arici, Muhammet [Namik Kemal University, Agricultural Faculty, Department of Food Engineering, 59030 Tekirdag (Turkey)

    2011-04-15

    Hazelnut, walnut, almonds, and pistachio nuts were treated with 1, 3, 5, and 7 kGy of gamma irradiation, respectively. Oil content, free fatty acid, peroxide value, and fatty acid composition of the nuts were investigated immediately after irradiation. The data obtained from the experiments indicated that gamma irradiation did not cause any significant change in the oil content of nuts. In contrast, free fatty acid and peroxide value of the nuts increased proportionally to the dose (p<0.05). Among the fatty acids determined, the concentration of total saturated fatty acids increased while total monounsaturated and total polyunsaturated fatty acids decreased with the irradiation dose (p<0.05 and <0.01).

  11. Validation of a multi-analyte HPLC-DAD method for determination of uric acid, creatinine, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid and 2-methylhippuric acid in human urine.

    Science.gov (United States)

    Remane, Daniela; Grunwald, Soeren; Hoeke, Henrike; Mueller, Andrea; Roeder, Stefan; von Bergen, Martin; Wissenbach, Dirk K

    2015-08-15

    During the last decades exposure sciences and epidemiological studies attracts more attention to unravel the mechanisms for the development of chronic diseases. According to this an existing HPLC-DAD method for determination of creatinine in urine samples was expended for seven analytes and validated. Creatinine, uric acid, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid, and 2-methylhippuric acid were separated by gradient elution (formate buffer/methanol) using an Eclipse Plus C18 Rapid Resolution column (4.6mm×100mm). No interfering signals were detected in mobile phase. After injection of blank urine samples signals for the endogenous compounds but no interferences were detected. All analytes were linear in the selected calibration range and a non weighted calibration model was chosen. Bias, intra-day and inter-day precision for all analytes were below 20% for quality control (QC) low and below 10% for QC medium and high. The limits of quantification in mobile phase were in line with reported reference values but had to be adjusted in urine for homovanillic acid (45mg/L), niacinamide 58.5(mg/L), and indole-3-acetic acid (63mg/L). Comparison of creatinine data obtained by the existing method with those of the developed method showing differences from -120mg/L to +110mg/L with a mean of differences of 29.0mg/L for 50 authentic urine samples. Analyzing 50 authentic urine samples, uric acid, creatinine, hippuric acid, and 2-methylhippuric acid were detected in (nearly) all samples. However, homovanillic acid was detected in 40%, niacinamide in 4% and indole-3-acetic acid was never detected within the selected samples.

  12. Ion chromatographic determination of dibutylphosphoric acid in nuclear fuel reprocessing streams

    International Nuclear Information System (INIS)

    A rapid method was developed for the determination of dibutylphosphoric acid (DBP), a degradation product of tributylphosphate (TBP), which is used in a solvent extraction process for recovery of uranium. DBP, along with any monobutylphosphoric acid (MBP) and phosphoric acid, are extracted from the organic phase into dilute sodium hydroxide. DBP is separated from MBP and phosphoric acid by ion chromatography (IC) and is determined on a peak height ratio basis. The method required only 30 minutes per analysis as compared to the conventional alumina column separation-colorimetric determination procedure, which requires eight hours to complete. DBP has been quantified to a lower limit of 1.5 mg/l. Relative standard deviations ranging from 5.7 to 0.4% were obtained for DBP concentrations ranging from 1.5 to 500 mg/l, respectively

  13. The comparison of techniques and methods for L-ascorbic acid determination in the fruits

    Directory of Open Access Journals (Sweden)

    Cvetković Biljana R.

    2012-01-01

    Full Text Available Vitamin C is an essential vitamin for human nutrition; with the L-ascorbic acid (AA being the active form of vitamin C. Hence, determination of the L-ascorbic acid in the natural and processed foods is very important. In the past, plenty of methods based on the reversible redox reaction of AA oxidation/DHA reduction were developed. Because of L-ascorbic acid instability in aqueous solutions, it is useful to analyze various types of extraction. The aim of this study is to compare three different methods and three different extractants for the L-ascorbic acid determination. Fruits (kiwi, lemon, orange, and grapefruit were purchased from a local market. The L-ascorbic acid in these four samples was determined by the three different methods: the AOAC, the HPLC method with three different types of extractions, and the colorimetric method using ascorbate-oxidase. For the HPLC measurements, one part of the fruits was extracted with distilled water, the second with potassium hydrogen phosphate, and the third with 3% meta-phosphoric acid (MPA in 8% acetic acid. The HPLC measurements of each sample were repeated three times, the AOAC titration was repeated five times, and in the calorimetric method three measurements were performed. The results were statistically evaluated related to sample basis. Statistical analysis shows that there is a significant difference between the results for all three methods of extraction for all samples, except for the grapefruit sample where no significant difference was observed between the results obtained after the buffer extraction (E2 and the metaphosphoric acid in acetic acid extraction (E3. Discriminative analysis for the HPLC determinations proves that there is a clear difference and defined border between the samples in relation to the methods of extraction during the HPLC determination.

  14. A method for the determination of the dissociation constants of acids with an uncalibrated glass electrode

    NARCIS (Netherlands)

    Bos, M.; Lengton, W.

    1975-01-01

    A method is presented for the determination of absolute pKa values of acids in solvents with a high dielectric constant by potentiometry with an uncalibrated glass electrode; in the determination, the glass electrode becomes calibrated. The method has the advantage that it is rapid and simple. Moreo

  15. Simultaneous determination of 2-naphthoxyacetic acid and indole-3-acetic acid by first derivation synchronous fluorescence spectroscopy

    Science.gov (United States)

    Liu, Xiangxiang; Wan, Yiqun

    2013-07-01

    A simple, rapid, sensitive and selective method for simultaneously determining 2-naphthoxyacetic acid (BNOA) and Indole-3-Acetic Acid (IAA) in mixtures has been developed using derivation synchronous fluorescence spectroscopy based on their synchronous fluorescence. The synchronous fluorescence spectra were obtained with Δλ = 100 nm in a pH 8.5 NaH2PO4-NaOH buffer solution, and the detected wavelengths of quantitative analysis were set at 239 nm for BNOA and 293 nm for IAA respectively. The over lapped fluorescence spectra were well separated by the synchronous derivative method. Under optimized conditions, the limits of detection (LOD) were 0.003 μg/mL for BNOA and 0.012 μg/mL for IAA. This method is simple and expeditious, and it has been successfully applied to the determination of 2-naphthoxyacetic acid and indole-3-acetic acid in fruit juice samples with satisfactory results. The samples were only filtrated through a 0.45 μm membrane filter, which was free from the tedious separation procedures. The obtaining recoveries were in the range of 83.88-87.43% for BNOA and 80.76-86.68% for IAA, and the relative standard deviations were all less than 5.0%. Statistical comparison of the results with high performance liquid chromatography Mass Spectrometry (HPLC-MS) method revealed good agreement and proved that there were no significant difference in the accuracy and precision between these two methods.

  16. Simple and Rapid Method for the Determination of Uric Acid-Independent Antioxidant Capacity

    Directory of Open Access Journals (Sweden)

    Darko Modun

    2011-08-01

    Full Text Available Determination of the relative contribution of uric acid level increases to the total measured antioxidative activity could be very useful for testing antioxidative products and their effect on human health. The aim of this report is to present a simple spectrophotometric method that combines the measurement of total antioxidative capacity of a sample by ferric reducing/antioxidative power (FRAP assay, with the uricase-reaction (specific elimination of uric acid, in order to establish and correct for the contribution of uric acid in FRAP values. We measured FRAP values, with (uric acid-independent antioxidant capacity, TAC-UA and without (total antioxidant capacity, TAC uricase treatment, and expressed it as μmol/L of uric acid equivalents. In such way, it was possible to determine both total and uric acid-independent antioxidant capacity, plasma uric acid (UA, as the difference between TAC and TAC-UA, and the ratio of the uric acid in total antioxidant capacity (UA/TAC.

  17. Palyginamųjų daugiklių metodo taikymo nelikvidžiose rinkose galimybių vertinimas. Baltijos šalių atvejis

    OpenAIRE

    Vilkauskaitė, Gintarė

    2013-01-01

    Darbe analizuojamos palyginamųjų daugiklių metodo taikymo galimybės Baltijos šalių listinguojamoms įmonėms. Darbo tikslas - įvertinti palyginamųjų daugiklių metodo taikymo galimybes nelikvidžiose rinkose Baltijos šalių listinguojamų įmonių pavyzdžiu. Darbą sudaro trys dalys, kurių pirmojoje pristatomi daugiklių metodo privalumai, trūkumai, praktinio pritaikymo etapai ir skirtingų metodų, naudojamų kiekviename praktinio pritaikymo etape, poveikio vertinimo rezultatams apžvalga. Antroje dalyje ...

  18. Eletropolymerization of Niacinamide for Fabrication of Electrochemical Sensor: Simultaneous Determination of Dopamine, Uric Acid and Ascorbic Acid

    Institute of Scientific and Technical Information of China (English)

    ZHU Xiaohong; LIN Xiangqin

    2009-01-01

    Two polymeric thin film modified electrodes, poly-niacinamide/glassy carbon electrode (poly-NA/GCE) and poly-nicotinic acid/glassy carbon electrode (poly-NC/GCE), have be fabricated at glassy carbon electrodes by sim-ple electropolymerization of niacinamide (NA) in different potential scan ranges of cyclic voltammetry (CV). These two electrodes all showed catalytic ability towards the oxidation of dopamine (DA), uric acid (UA) and ascorbie acid (AA) by obvious reductions of overpotentials, giving well-resolved voltammetric peaks, which allow simulta-neously determination of DA, UA and AA. The poly-NC/GCE showed even higher electrocatalytic activity than the poly-NA/GCE. The electrochemical behavior of poly-NC/GCE was investigated by CV and differential pulse voltammetry (DPV) for determination of DA, UA and AA. The linear ranges of the concentration for the determination of AA, DA and UA using DPV were 75-3000, 0.37-16 and 0.741--230 μmol·L-1, respectively. The slopes of the linear calibration curves for the detection were estimated to be 5.6, 1140 and 102 mA·L·mol-1 for AA, DA and UA, respectively. The poly-NC/GCE shows excellent sensitivity, good selectivity and antifouling properties.

  19. Determination of naphthenic acids in crude oil by chemical ionization mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    L(U) Zhenbo; TIAN Songbai; ZHAI Yuchun; DING Yi; ZHUANG Lihong

    2005-01-01

    Naphthenic acids in petroleum are considered a class of biological markers. Their potential use in source correlation and as an indicator of biodegradation was reported in the past (Dzidic et al. ,1988; Behar and Albrecht, 1984). Due to their highly complicated properties, detailed characterization of the acids is difficult.A method based on positive ion CI (chemical ionization) mass spectrometry using isobutane reagent gas to produce (M + 15) + ions was applied to the analysis of naphthenic acid esters. Since the complex mixture of naphthenic acids cannot be separated into individual components, only the determination of relative distribution of acids classified in terms of hydrogen deficiency was possible. The identities and relative distribution of fatty and mono-, di-, tri-, and higher polycyclic acids were obtained from the intensities of the (M + 15) + ions according to z-series formula CnH2n+zO2 of naphthenic acids. The components are characterized on the basis of group type and carbon number distributions. A comparison of the FAB and CI results showed that the group type distributions obtained by both methods agree surprisingly well.The results indicated this method is simple, rapid and easy to operate. The geochemical implication of naphthenic acids was investigated by using a set of well-characterized crude oil samples. It is found that the naphthenic acid distribution can be used as a fingerprint for oil-oil and oil-source correlations.

  20. Trace determination of cobalt ion by using malic acid-malonic acid double substrate oscillating chemical system

    Institute of Scientific and Technical Information of China (English)

    Jie Wang; Wu Yang; Jie Ren; Miao Guo; Xiao Dong Chen; Wen Bin Wang; Jin Zhang Gao

    2008-01-01

    A novel kinetic method for determination of trace amounts of cobalt ion was proposed and validated. The method is based on adding malic acid into classical Belousov-Zhabotinskii (B-Z) oscillating chemical system to form a double substrate one. The results showed that when the concentration of cobalt ion was in the range of 5.27× 10-8 to 5.37×10-12mol L-1 the change of the oscillating period was directly proportional to the negative logarithm of cobalt ion concentration. The sensitivity and precision of the developed method were quite satisfactory. The limit of detection was down to 5.20 x 10-13 mol L-1 which was a highest sensitivity found for determination of metal ions using oscillating chemical reaction so far. Some factors influencing the determination were also examined. The method has been successfully used to determine cobalt ion in vitamin B12 injection.

  1. Multi-elemental analysis of atmospheric pollutants and determination of particle size using the PIXE method, a cascade impactor and a filter unit constructed in Mexico; Analisis multielemental de contaminantes atmosfericos y determinacion de tamano de particula utilizando el metodo PIXE, un impactor de cascada y una unidad de filtro construidos en Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Aldape U, F. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)

    1989-01-15

    This work presents: 1) The methodology and the experimental conditions of the PIXE technique so that it is used as a better option inside the analytical methods in aerosols studies, 2) The development, tests and applications of a cascade impactor of the Batelle type built to determine particle size to use it jointly with the mentioned technique in the determination of the elements concentration according to its size.By this way is fulfilled with the first goal of this extensive project. (Author)

  2. Chemiluminescence Determination of Benzoic Acid Using A Solid-Phase Verdigris Reactor

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A new chemiluminescence flow system has been developed for sequential determina-tion of benzoic acid based on the reaction of the compound with copper carbonate entrapped in a solid-phase reactor. It was found that the unsaturated complex of Cu(II) and benzoic acid (1:1) has strong catalytic effect on the luminol-H2O2 chemiluminescence reaction. The calibration graph is linear over the range of 0.025 ~ 60 μg/mL of benzoic acid, with a relative standard deviation of less than 3.0 %, and the detection limit is 0.01μg@mL-1. The proposed method was applied to the determination of benzoic acid content in different pharmaceutical formulations.

  3. Determination of aliphatic organic acids by high-performance liquid chromatography with pulsed electrochemical detection.

    Science.gov (United States)

    Casella, Innocenzo G; Gatta, Maria

    2002-01-01

    A new ion exclusion HPLC procedure accomplished with a pulsed electrochemical detection for the determination of several common aliphatic acids is described. A triple-step waveform of the applied potentials, based on the formation/inhibition of PtOH species on the electrode surface, is successfully used for sensitive detection of several aliphatic acids in flowing systems avoiding pre- or postcolumn derivatization and/or cleanup procedures. Under optimal chromatographic conditions (i.e., 50 mM HClO(4)) the proposed method allowed detection limits between 0.5 and 7 microM for all investigated acids, and the dynamic linear range spanned generally over 1 or 2 orders of magnitude. Determination of citric, malic, tartaric, lactic, formic, and acetic acids in several foods and beverages was performed, in approximately 15 min, without the necessity of any sample pretreatment. PMID:11754537

  4. Quantitative determination of citric acid in seminal plasma by using Raman spectroscopy.

    Science.gov (United States)

    Huang, Zufang; Chen, Xiwen; Li, Yongzeng; Chen, Jinhua; Lin, Juqiang; Wang, Jing; Lei, Jinping; Chen, Rong

    2013-07-01

    In this study, Raman spectroscopy was first used to study the linear relationship between Raman spectral intensities and citric acid concentrations in aqueous solution. By using the specific Raman band of 942 cm(-1), concentrations of citric acid ranging from 2 to 20 mg/mL were observed linearly (R(2) = 0.993), and the limit of detection was 1.0 mg/mL. Then, citric acid detection in clinical seminal plasma ultrafiltrate samples was performed, and the intensity of the Raman-specific peak demonstrates a good linear correlation (R(2) = 0.946) with citric acid concentrations determined by the enzymatic method. Our results showed that Raman spectroscopy has the potential of being applied to detect concentrations of citric acid in seminal plasma in clinic.

  5. Determination of uranium content in phosphoric and sulfuric acids used by the phosphatized fertilizers industry

    International Nuclear Information System (INIS)

    Uranium content in phosphoric and sulfuric acids is determined. The uranium was measured through the fission track registration technique, using Makrofol KG, 10 μg thick, as detector. The so-called 'wet' method was adopted and the acid samples were used directly as irradiation medium. This proceeding showed the advantages of simple sample preparation and avoided the need of changing the acid samples media to nitric medium, as commonly used. The analysis of the sulfuric acid samples showed uranium contents under the detection limit of the technique (4 ppb). The results found for phosphoric acid samples ranged from 31 to 845 ppm, with experimental errors between 7.9 and 9.7%. (Author)

  6. Determination of the Fatty Acid content of pumpkin seed, pygeum, and saw palmetto.

    Science.gov (United States)

    Ganzera, M; Croom, E M; Khan, I A

    1999-01-01

    Fatty acids are major components of many plants, foods and medicines, including pumpkin seeds (Cucubita pepo), pygeum bark (Prunus africana) and saw palmetto (Serenoa repens). With the gas chromatography methods reported here, free fatty acids of these species can be quantified as their trimethylsilyl derivatives. Because of their different fatty acid contents and composition, the gas chromatography method can distinguish which of three plant species was extracted, and, in the case of S. repens, the method of extraction. Although phytosterols can be separated by this method, their content is too low to be assigned directly. The total fatty acid content can be determined through formation of the methyl esters. This is helpful for estimation of the kind and percentage of fatty acids that are present as triglyceride esters in the plant material and for standardization of the products.

  7. Determination of surface-accessible acidic hydroxyls and surface area of lignin by cationic dye adsorption

    OpenAIRE

    Sipponen, Mika Henrikki; Pihlajaniemi, Ville; Littunen, Kuisma; Pastinen, Ossi; Laakso, Simo

    2014-01-01

    A new colorimetric method for determining the surface-accessible acidic lignin hydroxyl groups in lignocellulose solid fractions was developed. The method is based on selective adsorption of Azure B, a basic dye, onto acidic hydroxyl groups of lignin. Selectivity of adsorption of Azure B on lignin was demonstrated using lignin and cellulose materials as adsorbents. Adsorption isotherms of Azure B on wheat straw (WS), sugarcane bagasse (SGB), oat husk, and isolated lignin materials were determ...

  8. Determination of ascorbic acid in pharmaceutical preparation and fruit juice using modified carbon paste electrode

    OpenAIRE

    Simona Žabčíková; Dai Long Vu; Libor Červenka; Vojtěch Tambor; Martina Vašatová

    2016-01-01

    Acrobic acid is key substance in the human metabolism and the rapid and accurate determination in food is of a great interest. Ascorbic acid is an electroactive compound, however poorly responded on the bare carbon paste electrodes. In this paper, brilliant cresyl blue and multi-walled carbon nanotubes were used for the modification of carbon paste electrode. Brilliant cresyl blue acts as a mediator improving the transition of electrons, whereas multiwalled carbon nanotubes increased the surf...

  9. Determination of Kr-85 in environmental samples and gaseous effluents from nuclear industries using the standard method; Aplicacion del metodo de concentracion separacion y medida radiactiva por centelleo liquido de Kr-85 en muestras ambientales y en efluentes gaseosos de la industria nuclear

    Energy Technology Data Exchange (ETDEWEB)

    Heras, M. c.; Perez, M. M.

    1983-07-01

    The determination of the Kr-85 activity in environmental samples and gaseous effluents from Spanish Nuclear Power Stations is described. The method employed has been published elsewhere. The determinations has been carried out in environmental samples token at JEN Laboratories (Madrid) and the Nuclear Power Stations, Jose Cabrera (Zorita), Garona and Vandellos. Also samples of gaseous effluents of the three plants has been analyzed. Values of the Kr-85 environmental background activity in the Almaraz Nuclear Power Stations, has been determined, before the beginning of its nuclear activity. In this paper the sampling equipment used is described and the values found of Kr-85 activity in all the samples in given. (Author) 29 refs.

  10. Determination of water-soluble forms of oxalic and formic acids in soils by ion chromatography

    Science.gov (United States)

    Karicheva, E.; Guseva, N.; Kambalina, M.

    2016-03-01

    Carboxylic acids (CA) play an important role in the chemical composition origin of soils and migration of elements. The content of these acids and their salts is one of the important characteristics for agrochemical, ecological, ameliorative and hygienic assessment of soils. The aim of the article is to determine water-soluble forms of same carboxylic acids — (oxalic and formic acids) in soils by ion chromatography with gradient elution. For the separation and determination of water-soluble carboxylic acids we used reagent-free gradient elution ion-exchange chromatography ICS-2000 (Dionex, USA), the model solutions of oxalate and formate ions, and leachates from soils of the Kola Peninsula. The optimal gradient program was established for separation and detection of oxalate and formate ions in water solutions by ion chromatography. A stability indicating method was developed for the simultaneous determination of water-soluble organic acids in soils. The method has shown high detection limits such as 0.03 mg/L for oxalate ion and 0.02 mg/L for formate ion. High signal reproducibility was achieved in wide range of intensities which correspond to the following ion concentrations: from 0.04 mg/g to 10 mg/L (formate), from 0.1 mg/g to 25 mg/L (oxalate). The concentration of formate and oxalate ions in soil samples is from 0.04 to 0.9 mg/L and 0.45 to 17 mg/L respectively.

  11. Simultaneous determination of rutin and ascorbic acid mixture in their pure forms and combined dosage form.

    Science.gov (United States)

    Attia, Tamer Z

    2016-12-01

    A simple, rapid, sensitive and selective high performance liquid chromatographic (HPLC) method with ultraviolet detection has been developed for simultaneous determination of ascorbic acid and rutin in pure forms and pharmaceutical dosage form. HPLC separation was performed on Phenomenex C18 analytical column with 0.1% v/v acetic acid in water and acetonitrile (75:25, v/v), as mobile phase. The separation was done at ambient temperature with flow rate of 1mL·min(-1) in isocratic mode. HPLC measurements were carried out using ultraviolet detection wavelength at 257nm. The average retention times were 2.72 and 7.00min for ascorbic acid and rutin, respectively. The calibration plots were constructed over the concentration range of 5.0-30.0 for ascorbic acid and 10.0-60.0μg·mL(-1) for rutin. The limits of detection were 1.06 and 1.89μg·mL(-1) and limits of quantification were 3.54 and 6.31μg·mL(-1) for ascorbic acid and rutin, respectively. The proposed HPLC-UV method was successfully applied for determination of ascorbic acid in its tablets and for simultaneous determination of the studied drugs in their laboratory prepared mixtures and in pharmaceutical formulation. Statistical comparisons of the results with the reference method show an excellent agreement and indicate no significant difference in respect to accuracy and precision. PMID:27341400

  12. Flow-injection Spectrophotometric Determination of Uric Acid in Urine via Prussian Blue Reaction

    Institute of Scientific and Technical Information of China (English)

    WASEEM Amir; YAQOOB Mohammad; NABI Abdul; MURTAZA Ghulam; HUSSAIN Izhar

    2011-01-01

    A simple and sensitive flow injection(FI)spectrophotometric method was reported for the determination of uric acid based on the reduction of Fe(Ⅲ)/ferricyanide in the presence of uric acid.The in situ reduced ions reacted with unreduced portion of ferricyanide/Fe(Ⅲ)to form soluble Prussian blue,which was monitored at an absorption wavelength of 735 nm.The optimized conditions allow a linear calibration graph in a concentration range of 1-100μmol/L.The relative standard deviation was in a range of 0.5%-2.5%,with a detection limit(3σ blank)of 0.3 μmol/L and a sampling frequency of 60 injection/h was obtained.The effect of common substances present in human physiological fluids on the determination of uric acid was examined.The method was applied to determining uric acid in human urine samples with the recoveries in a range of 96%-105%.The results agree well with those by spectrophotometric reference method at a confidence level of 95%.Spectrophotometric procedures for uric acid determination in clinical samples were reviewed briefly.

  13. Determination of fatty acid profile in ram spermatozoa and seminal plasma.

    Science.gov (United States)

    Díaz, R; Torres, M A; Bravo, S; Sanchez, R; Sepúlveda, N

    2016-08-01

    Fatty acids are important in male reproductive function because they are associated with membrane fluidity, acrosome reaction, sperm motility and viability, but limited information exists about the fatty acid profile of ram semen. Our aim was to determine the fatty acid composition in ram spermatozoa and seminal plasma. Sixty ejaculates were obtained from three ram (20 ejaculates/ram) using artificial vagina. Ram spermatozoa (RS) and seminal plasma (SP) were separated using centrifugation, and the fatty acids were analysed by gas chromatography. Total lipids obtained in ram spermatozoa were 1.8% and 1.6% in seminal plasma. Saturated fatty acid (SFA) was proportionally major in SP (66.6%) that RS (49.9%). The highest proportions of SFA corresponded to C4:0 (RS = 16.3% and SP = 28.8%) and C16:0 (RS = 16.3% and PS = 20%). The most important unsaturated fatty acid (UFA) was docosahexaenoic acid (DHA), 44.9% in RS and 31.5% in SP. The profile of fatty acid and their proportions showed differences between spermatozoa and seminal plasma.

  14. Comparative Study of the Total Acidity Determination in Wine by Potentiometric and Volumetric Titration

    OpenAIRE

    Budić-Leto, Irena; Mešin, Nela; Gajdoš Kljusurić, Jasenka; Pezo, Ivan; Bralić, Marija

    2009-01-01

    Total acidity was determined in thirty-seven samples of Croatian red, white and rosé wines by potentiometric titration. In order to find the effect of the corresponding rate of the automatic titrant added, several procedures were employed. For different rates of titration, the aberrances were found from 0.1 to 0.4 g L–1 for some wines. The value of the total acid content in wine determined by the automatic potentiometric titration method was compared to that obtained by the conventional volum...

  15. Determination of gallic acid with rhodanine by reverse flow injection analysis using simplex optimization.

    Science.gov (United States)

    Phakthong, Wilaiwan; Liawruangrath, Boonsom; Liawruangrath, Saisunee

    2014-12-01

    A reversed flow injection (rFI) system was designed and constructed for gallic acid determination. Gallic acid was determined based on the formation of chromogen between gallic acid and rhodanine, resulting in a colored product with a λmax at 520 nm. The optimum conditions for determining gallic acid were also investigated. Optimizations of the experimental conditions were carried out based on the so-call univariate method. The conditions obtained were 0.6% (w/v) rhodanine, 70% (v/v) ethanol, 0.9 mol L(-1) NaOH, 2.0 mL min(-1) flow rate, 75 μL injection loop and 600 cm mixing tubing length, respectively. Comparative optimizations of the experimental conditions were also carried out by multivariate or simplex optimization method. The conditions obtained were 1.2% (w/v) rhodanine, 70% (v/v) ethanol, 1.2 mol L(-1) NaOH, flow rate 2.5 mL min(-1), 75 μL injection loop and 600 cm mixing tubing length, respectively. It was found that the optimum conditions obtained by the former optimization method were mostly similar to those obtained by the latter method. The linear relationship between peak height and the concentration of gallic acid was obtained over the range of 0.1-35.0 mg L(-1) with the detection limit 0.081 mg L(-1). The relative standard deviations were found to be in the ranges 0.46-1.96% for 1, 10, 30 mg L(-1) of gallic acid (n=11). The method has the advantages of simplicity extremely high selectivity and high precision. The proposed method was successfully applied to the determination of gallic acid in longan samples without interferent effects from other common phenolic compounds that might be present in the longan samples collected in northern Thailand. PMID:25159449

  16. Influence of tryptophan loading on urinary excretion of anthranilic acid and 3-hydroxyanthranilic acid by men and women as determined by alkali flame ionization gas chromatography

    NARCIS (Netherlands)

    Poll, J.M. van der; Vink, M.; Schrijver, J.; Odink, J.

    1986-01-01

    A gas chromatographic method with alkali flame ionization detection is described for the determination of urinary total (free and conjugated) anthranilic acid (AA) and 3-hydroxyanthranilic acid (HAA) as their pentafluorobenzyl esters. Prior to analysis, urine was hydrolysed using hydrochloric acid i

  17. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-12-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  18. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-02-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  19. Are the Crystal Structures of Enantiopure and Racemic Mandelic Acids Determined by Kinetics or Thermodynamics?

    Science.gov (United States)

    Hylton, Rebecca K; Tizzard, Graham J; Threlfall, Terence L; Ellis, Amy L; Coles, Simon J; Seaton, Colin C; Schulze, Eric; Lorenz, Heike; Seidel-Morgenstern, Andreas; Stein, Matthias; Price, Sarah L

    2015-09-01

    Mandelic acids are prototypic chiral molecules where the sensitivity of crystallized forms (enantiopure/racemic compound/polymorphs) to both conditions and substituents provides a new insight into the factors that may allow chiral separation by crystallization. The determination of a significant number of single crystal structures allows the analysis of 13 enantiopure and 30 racemic crystal structures of 21 (F/Cl/Br/CH3/CH3O) substituted mandelic acid derivatives. There are some common phenyl packing motifs between some groups of racemic and enantiopure structures, although they show very different hydrogen-bonding motifs. The computed crystal energy landscape of 3-chloromandelic acid, which has at least two enantiopure and three racemic crystal polymorphs, reveals that there are many more possible structures, some of which are predicted to be thermodynamically more favorable as well as slightly denser than the known forms. Simulations of mandelic acid dimers in isolation, water, and toluene do not differentiate between racemic and enantiopure dimers and also suggest that the phenyl ring interactions play a major role in the crystallization mechanism. The observed crystallization behavior of mandelic acids does not correspond to any simple "crystal engineering rules" as there is a range of thermodynamically feasible structures with no distinction between the enantiopure and racemic forms. Nucleation and crystallization appear to be determined by the kinetics of crystal growth with a statistical bias, but the diversity of the mandelic acid crystallization behavior demonstrates that the factors that influence the kinetics of crystal nucleation and growth are not yet adequately understood.

  20. DETERMINATION OF Cu, Fe, Mn, Zn AND FREE FATTY ACIDS IN PEQUI OIL

    Directory of Open Access Journals (Sweden)

    Aparecida M. S. Mimura

    2016-06-01

    Full Text Available Pequi (Caryocar brasiliense Camb., a typical fruit of the Brazilian Cerrado, is an important source of micronutrients and fatty acids. In this work, a new approach for the acid digestion (using H2SO4, HNO3 and H2O2 of pequi oil samples and the determination of Cu, Fe, Zn and Mn by flame atomic absorption spectrometry (F AAS was employed. Capillary zone electrophoresis (CZE was used for free fatty acid (FFA determination after simple and fast extraction with heated ethanol. Good results regarding precision (RSD < 10%, in most cases, sensitivity and adequate LOD and LOQ values were obtained. The accuracy was evaluated using spike tests and the recoveries were from 97 to 107%. The analytes were investigated in four different pequi oil samples. Fe was the trace element with the highest concentration (from 1.99 to 10.3 mg/100 g, followed by Zn, Mn and Cu (1.15 to 3.19, 0.42 to 0.91 and 0.31 to 0.56 mg/100 g, respectively. The main FFA found were oleic acid and palmitic acid (1.61 to 10.7 and 0.82 to 2.69 g/100 g, respectively, while linoleic acid (0.50 g/100 g was detected in only one sample. The pequi oil chemical composition showed good characteristics to be used as a food additive, in cosmetic formulations and for traditional medicine.

  1. Separative determination of ascorbic acid analogs contained in mushrooms by high-performance liquid chromatography.

    Science.gov (United States)

    Okamura, M

    1998-02-01

    Analogs (6-deoxyascorbic acid, erythroascorbic acid, and associated glycosides) of L-ascorbic acid (AA) contained in mushrooms were allowed to react with hydrazine to form osazones, and the conditions for separative determination by HPLC using a Zorbax SIL column were examined. Separation was started using solvent system 1 (ethylacetate/n-hexane/acetone/acetic acid, 50:50:1:1, v/v) as the mobile phase, and switching after 15 min to solvent system 2 (ethylacetate/acetone/acetic acid, 100:1:1, v/v). Detection was performed by absorbance at 500 nm. Because these analogs showed different formation rates for osazone, calibration curves were prepared for each substance. The recovery rate in the load test was 93-105%. By this method, AA and the analogs contained in eight species of edible mushrooms have been determined. The results revealed that: (1) the main constituents of all mushrooms are AA analogs rather than AA itself; (2) only one species contained AA in a very small amount (2 mumol/kg); (3) the types of AA analogs present differed according to the species of mushrooms, and (4) the total amount of AA analogs was between ca. 100-500 mumol/kg (2-9 mg per 100 g, converted to AA). In addition, a new AA analog was found in Pleurotus ostreatus and identified as 5-O-(alpha-D-xylopyranosyl)-D-erythroascorbic acid in structural analyses by NMR and other methods. PMID:9591231

  2. Optimization of the Analytical Method Using HPLC with Fluorescence Detection to Determine Selected Polycyclic Aromatic Compounds in Clean Water Samples; Optimizacion del Metodo Analitico mediante HPLC con Detector de Fluorescencia para la Determinacion de Ciertos Compuestos Aromaticos Policiclicos en Muestras de Aguas Limpias

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.

    2013-10-01

    A study on the comparison and evaluation of 3 miniaturized extraction methods for the determination of selected PACs in clear waters is presented. Three types of liquid-liquid extraction were used for chromatographic analysis by HPLC with fluorescence detection. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the scope of the methods developed at low and high levels of concentration and intermediate precision. (Author)

  3. Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode.

    Science.gov (United States)

    Veera Manohara Reddy, Y; Prabhakara Rao, V; Vijaya Bhaskar Reddy, A; Lavanya, M; Venu, M; Lavanya, M; Madhavi, G

    2015-12-01

    In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1M phosphate buffer solution (PBS) at pH7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 μM over the linear dynamic range of 1.6 μM to 16 μM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples. PMID:26354279

  4. Simultaneous determination of C2-C22 non-esterified fatty acids and other metabolically relevant carboxylic acids in biological material by gas chromatography of their benzyl esters.

    Science.gov (United States)

    Schatowitz, B; Gercken, G

    1988-03-18

    A method for the simultaneous determination of non-esterified short-, medium- and long-chain fatty acids and other types of metabolically relevant carboxylic acids such as hydroxy, keto, aromatic and dicarboxylic acids in biological material by capillary gas chromatography of benzyl ester derivatives is described. Sample preparation avoiding incomplete isolation of carboxylic acids consisted of deproteinization and extraction with ethanol, fixation of carboxylic acids as carboxylates, removal of interfering compounds such as neutral lipids by hexane extraction and amino acids, acyl carnitines and other cations by cation-exchange chromatography, derivatization of keto groups of ketocarboxylic acids into O-methyl oximes and benzyl ester formation by reaction of the potassium carboxylates with benzyl bromide via crown ether catalysis. The sample preparation conditions were investigated, showing the usefulness of this method for quantitative determinations. Chromatograms obtained from human serum, human urine and rat heart ventricle and concentrations of carboxylic acids in these specimens are presented. PMID:3372640

  5. Determination of surface-accessible acidic hydroxyls and surface area of lignin by cationic dye adsorption.

    Science.gov (United States)

    Sipponen, Mika Henrikki; Pihlajaniemi, Ville; Littunen, Kuisma; Pastinen, Ossi; Laakso, Simo

    2014-10-01

    A new colorimetric method for determining the surface-accessible acidic lignin hydroxyl groups in lignocellulose solid fractions was developed. The method is based on selective adsorption of Azure B, a basic dye, onto acidic hydroxyl groups of lignin. Selectivity of adsorption of Azure B on lignin was demonstrated using lignin and cellulose materials as adsorbents. Adsorption isotherms of Azure B on wheat straw (WS), sugarcane bagasse (SGB), oat husk, and isolated lignin materials were determined. The maximum adsorption capacities predicted by the Langmuir isotherms were used to calculate the amounts of surface-accessible acidic hydroxyl groups. WS contained 1.7-times more acidic hydroxyls (0.21 mmol/g) and higher surface area of lignin (84 m(2)/g) than SGB or oat husk materials. Equations for determining the amount of surface-accessible acidic hydroxyls in solid fractions of the three plant materials by a single point measurement were developed. A method for high-throughput characterization of lignocellulosic materials is now available. PMID:25033327

  6. Determination of the ratio of the spectral fluence of electrons in water, using a Newton Cotes closed quadrature method: rule composed of trapezium with non equi-spaced nodes; Determinacion de la razon de fluencias espectrales de electrones en agua, usando un metodo de cuadratura cerrada de Newton Cotes: regla compuesta del trapecio con nodos no equi-espaciados

    Energy Technology Data Exchange (ETDEWEB)

    Moranchel y Rodriguez, M. [IPN, ESFM, Departamento de Ingenieria Nuclear, 07738 Mexico D.F. (Mexico)]. e-mail: mmoranchel@ipn.mx

    2008-07-01

    The central problem of the dosimetry of the ionizing radiations is the determination of the dissipated energy by unit of mass of irradiated material. This energy usually is inferred of ionization measures in a small cavity of air housed inside the material medium. The Bragg-Gray cavity theory was the first one in estimating the dissipated energy through the ionizations that the primary electrons cause in the cavity. The primary electrons are generated by photoelectric effect, pair production and by Compton dispersion of the photon beams that initially impact on the material. However, in a more realist approach the existence of secondary electrons due to the electron-electron interaction it will be considered. The Spencer-Attix cavity theory considers to the secondary electrons as responsible part for the energy deposited in the means, for that a total spectral fluence of electrons (primary and secondary) it appears in this theory. Few electrons spectra have been published, mainly, those that include the contribution of secondary electrons ({delta} rays). Leaving of the ideas of Spencer-Attix, in this work an approach method to determine the rate of electron spectral fluences (total regarding primary) for a wide variety of material Z, and energy sources T{sub 0} is presented. The method for materials used by Spencer-Attix is applied, it is proven its reliability and it is applied to the water like absorber medium by its importance in the clinical dosimetry. (Author)

  7. Determination of {sup 60} Co by means of Neutron Activation Analysis in the sorption of Co in synthesized porous oxides by the combustion method; Determinacion de {sup 60} Co por medio de AAN en la sorcion de Co en oxidos porosos sintetizados por metodo de combustion

    Energy Technology Data Exchange (ETDEWEB)

    Lugo, V.; Bulbulian, S.; Urena, F. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)]. e-mail: violelugo@yahoo.es

    2005-07-01

    Recently inorganic materials are investigating as sorbent of radioactive pollutants present in water. The inorganic oxides belong to this group of materials. A quick method exists for the obtaining of inorganic oxides, denominated combustion method that could be used to produce porous oxides successfully with good properties for the sorption of radioactive ions. In this investigation, iron oxides, magnesium and zinc were synthesized obtained by the combustion method, comparing them with those synthesized by the calcination method, using two different synthesis temperatures. The obtained solids were characterized by scanning electron microscopy (Sem), by X-ray diffraction (XRD) and by semiquantitative elemental analysis (EDS). After the characterization, the crystalline oxides synthesized by both methods, to temperature of 800 C, were evaluated as sorbents in the removal of Co{sup 2+} ions, through experiments in batch, and using neutron activation analysis, determining the sorption percentage, with this it was concluded that the magnesium oxide produced by combustion it is more effective in the removal of Co{sup 2+} ions than that synthesized by calcination. It was determined the surface area of the magnesium oxides, obtaining a surface area greater for the synthesized oxide by combustion method. (Author)

  8. Flow-injection chemiluminescence determination of tryptophan using galangin-potassium permanganate-polyphosphoric acid system

    Institute of Scientific and Technical Information of China (English)

    Hui Chen; Li Li; Min Zhou; Yong Jun Ma

    2008-01-01

    A high sensitive flow-injection chemiluminescence (FI-CL)method for the determination of tryptephan has been developed.The method is based on the chemiluminescence reaction of galangin-potassium perrnanganate-tryptophan in polyphosphoric acid (PPA)media.Under the optimized conditions,tryptophan was determined in the range 0.05-10 μg/mL with the detection limit (30)of 5.0× 10-3 μg/mL.The relative standard deviation (RSD)was 1.0% for 11 replicate determinations of 1.0 μg/mL tryptophan.Three synthetic samples were determined selectively with recoveries in the range from 99.6% to 102.0% in the presence of other amino acids.

  9. Determination of fatty acid composition and quality characteristics of oils from palm fruits using solvent extraction

    Science.gov (United States)

    Kasmin, Hasimah; Lazim, Azwan Mat; Awang, Roila

    2015-09-01

    Palm oil contains about 45% of saturated palmitic acid and 39% of mono-unsaturated oleic acid. Investigations made in the past to trace the fatty acid composition in palm revealed that ripeness of fresh fruit bunch (FFB) affect oil composition. However, there is no evidence that processing operations affect oil composition, although different stage of processing does affect the quality of oil extracted. An improved method for sterilizing the oil palm fruits by dry heating, followed by oil extraction has been studied. This method eliminates the use of water, thus, increasing the extraction of lipid soluble. The objective of this study is to determine the possibility production of palm oil with different fatty acid composition (FAC) as well as the changes in quality from conventional milling. The unripe and ripe FFB were collected, sterilized and extracted using different method of solvent extraction. Preliminary data have shown that variation in FAC will also alter the physical and chemical properties of the oil extracted.

  10. Amino acids analysis by total neutron cross-sections determinations: part V

    Energy Technology Data Exchange (ETDEWEB)

    Voi, Dante L.; Ferreira, Francisco de O., E-mail: dante@ien.gov.br, E-mail: fferreira@ien.gov.br [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil); Rocha, Helio F. da, E-mail: helionutro@hotmail.com [Universidade Federal do Rio de Janeiro (IPPMG/UFRJ), Rio de Janeiro, RJ (Brazil). Instituto de Pediatria

    2013-07-01

    Total neutron cross-sections of twenty essential and non-essential amino acids to human were determined using crystal spectrometer installed on the Argonauta reactor of IEN (Instituto de Engenharia Nuclear (CNEN-RJ) and compared with data generated by parceling and grouping methodologies developed at this institution. For each amino acid was calculated the respective neutron cross-section by molecular structure, conformation and chemistry analysis. The results obtained for eighteen of twenty amino acids confirm the specifications and product formulations indicated by manufactures. These initial results allow to build a neutron cross-sections database as part of quality control of the amino supplied to hospitals for production of nutriments for parenteral or enteral formulations used in critical patients dependent on artificial feed, and for application in future studies of structure and dynamics for more complex molecules, including proteins, enzymes, fatty acids, membranes, organelles and other cell components. (author)

  11. Rapid determination of amino acids in biological samples using a monolithic silica column.

    Science.gov (United States)

    Song, Yanting; Funatsu, Takashi; Tsunoda, Makoto

    2012-05-01

    A high-performance liquid chromatography method in which fluorescence detection is used for the simultaneous determination of 21 amino acids is proposed. Amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) and then separated on a monolithic silica column (MonoClad C18-HS, 150 mm×3 mm i.d.). A mixture of 25 mM citrate buffer containing 25 mM sodium perchlorate (pH 5.5) and acetonitrile was used as the mobile phase. We found that the most significant factor in the separation was temperature, and a linear temperature gradient from 30 to 49°C was used to control the column temperature. The limits of detection and quantification for all amino acids ranged from 3.2 to 57.2 fmol and 10.8 to 191 fmol, respectively. The calibration curves for the NBD-amino acid had good linearity within the range of 40 fmol to 40 pmol when 6-aminocaproic acid was used as an internal standard. Using only conventional instruments, the 21 amino acids could be analyzed within 10 min. This method was found to be suitable for the quantification of the contents of amino acids in mouse plasma and adrenal gland samples.

  12. Paper-based electroanalytical devices for in situ determination of salicylic acid in living tomato leaves.

    Science.gov (United States)

    Sun, Li-Jun; Feng, Qiu-Mei; Yan, Yong-Feng; Pan, Zhong-Qin; Li, Xiao-Hui; Song, Feng-Ming; Yang, Haibing; Xu, Jing-Juan; Bao, Ning; Gu, Hai-Ying

    2014-10-15

    Detection of phytohormones in situ has gained significant attention due to their critical roles in regulating developmental processes and signaling for defenses in plants at low concentration. As one type of plant hormones, salicylic acid has recently been found to be one of pivotal signal molecules for physiological behaviors of plants. Here we report the application of paper-based electroanalytical devices for sensitively in situ detection of salicylic acid in tomato leaves with the sample volume of several microliters. Specifically, disposable working electrodes were fabricated by coating carbon tape with the mixture of multiwall carbon nanotubes and nafion. We observed that the treatment of the modified carbon tape electrodes with oxygen plasma could significantly improve electrochemical responses of salicylic acid. The tomato leaves had a punched hole of 1.5mm diameter to release salicylic acid with minor influence on continuous growth of tomatoes. By incorporating the tomato leaf with the paper-based analytical device, we were able to perform in situ determination of salicylic acid based on its electrocatalytic oxidation. Our experimental results demonstrated that the amounts of salicylic acid differed statistically in normal, phytoene desaturase (PDS) gene silent and diseased (infected by Botrytis cinerea) tomato leaves. By quantifying salicylic acid at the level of several nanograms in situ, the simple paper-based electroanalytical devices could potentially facilitate the study of defense mechanism of plants under biotic and abiotic stresses. This study might also provide a sensitive method with spatiotemporal resolution for mapping of chemicals released from living organisms. PMID:24794407

  13. Paper-based electroanalytical devices for in situ determination of salicylic acid in living tomato leaves.

    Science.gov (United States)

    Sun, Li-Jun; Feng, Qiu-Mei; Yan, Yong-Feng; Pan, Zhong-Qin; Li, Xiao-Hui; Song, Feng-Ming; Yang, Haibing; Xu, Jing-Juan; Bao, Ning; Gu, Hai-Ying

    2014-10-15

    Detection of phytohormones in situ has gained significant attention due to their critical roles in regulating developmental processes and signaling for defenses in plants at low concentration. As one type of plant hormones, salicylic acid has recently been found to be one of pivotal signal molecules for physiological behaviors of plants. Here we report the application of paper-based electroanalytical devices for sensitively in situ detection of salicylic acid in tomato leaves with the sample volume of several microliters. Specifically, disposable working electrodes were fabricated by coating carbon tape with the mixture of multiwall carbon nanotubes and nafion. We observed that the treatment of the modified carbon tape electrodes with oxygen plasma could significantly improve electrochemical responses of salicylic acid. The tomato leaves had a punched hole of 1.5mm diameter to release salicylic acid with minor influence on continuous growth of tomatoes. By incorporating the tomato leaf with the paper-based analytical device, we were able to perform in situ determination of salicylic acid based on its electrocatalytic oxidation. Our experimental results demonstrated that the amounts of salicylic acid differed statistically in normal, phytoene desaturase (PDS) gene silent and diseased (infected by Botrytis cinerea) tomato leaves. By quantifying salicylic acid at the level of several nanograms in situ, the simple paper-based electroanalytical devices could potentially facilitate the study of defense mechanism of plants under biotic and abiotic stresses. This study might also provide a sensitive method with spatiotemporal resolution for mapping of chemicals released from living organisms.

  14. Atomic Absorption and Spectrophotometeric Determinations of Salicylhydroxamic Acid in Its Pure and Pharmaceutical Dosage Forms

    OpenAIRE

    SALEM, Alaa-Eldin AbdelAziz

    2003-01-01

    A new method for the indirect determination of salicylhydroxamic acid (SHAM) using atomic absorption spectrometry (AAS) was proposed. The method is based on precipitating the ion associate complex of SHAM with [Cu (NH3)4]2+. The excess, unreacted, Cu2+ ions were determined using AAS. Another spectrophotometric method based on measuring the absorbance of the formed [Cu (NH3)4]-SHAM complex in dioxane was proposed. The green color of the complex formed was measured at 330 nm. The two...

  15. Voltammetric Determination of Ferulic Acid Using Polypyrrole-Multiwalled Carbon Nanotubes Modified Electrode with Sample Application

    Directory of Open Access Journals (Sweden)

    Refat Abdel-Hamid

    2015-10-01

    Full Text Available A polypyrrole-multiwalled carbon nanotubes modified glassy carbon electrode-based sensor was devised for determination of ferulic acid (FA. The fabricated sensor was prepared electrochemically using cyclic voltammetry (CV and characterized using CV and scanning electron microscope (SEM. The electrode shows an excellent electrochemical catalytic activity towards FA oxidation. Under optimal conditions, the anodic peak current correlates linearly to the FA concentration throughout the range of 3.32 × 10−6 to 2.59 × 10−5 M with a detection limit of 1.17 × 10−6 M (S/N = 3. The prepared sensor is highly selective towards ferulic acid without the interference of ascorbic acid. The sensor applicability was tested for total content determination of FA in a commercial popcorn sample and showed a robust functionality.

  16. Comparative Study of the Total Acidity Determination in Wine by Potentiometric and Volumetric Titration

    Directory of Open Access Journals (Sweden)

    Irena Budić-leto

    2009-03-01

    Full Text Available Total acidity was determined in thirty-seven samples of Croatian red, white and rosé wines by potentiometric titration. In order to find the effect of the corresponding rate of the automatic titrant added, several procedures were employed. For different rates of titration, the aberrances were found from 0.1 to 0.4 g L–1 for some wines. The value of the total acid content in wine determined by the automatic potentiometric titration method was compared to that obtained by the conventional volumetric titration method. The ANOVA and cluster analysis (CA were applied to detect possible resemblance. The results of total acidity depended on the methods used. However, a good correlation between the results by these methods was found.

  17. Ascorbic Acid Determination in Commercial Fruit Juice Samples by Cyclic Voltammetry

    Science.gov (United States)

    Pisoschi, Aurelia Magdalena; Danet, Andrei Florin; Kalinowski, Slawomir

    2008-01-01

    A method was developed for assessing ascorbic acid concentration in commercial fruit juice by cyclic voltammetry. The anodic oxidation peak for ascorbic acid occurs at about 490 mV on a Pt disc working electrode (versus SCE). The influence of the potential sweep speed on the peak height was studied. The obtained calibration graph shows a linear dependence between peak height and ascorbic acid concentration in the domain (0.1–10 mmol·L−1). The equation of the calibration graph was y = 6.391x + 0.1903 (where y represents the value of intensity measured for the anodic peak height, expressed as μA and x the analyte concentration, as mmol·L−1, r2 = 0.9995, r.s.d. = 1.14%, n = 10, Cascorbic acid = 2 mmol·L−1). The developed method was applied to ascorbic acid assessment in fruit juice. The ascorbic acid content determined ranged from 0.83 to 1.67 mmol·L−1 for orange juice, from 0.58 to 1.93 mmol·L−1 for lemon juice, and from 0.46 to 1.84 mmol·L−1 for grapefruit juice. Different ascorbic acid concentrations (from standard solutions) were added to the analysed samples, the degree of recovery being comprised between 94.35% and 104%. Ascorbic acid determination results obtained by cyclic voltammetry were compared with those obtained by the volumetric method with dichlorophenol indophenol. The results obtained by the two methods were in good agreement. PMID:19343183

  18. Development of potentiometric sensors for determining the concentration of ethan-1,2-dicarboxylic and 2-hydroxybenzoic acids

    OpenAIRE

    Matorina, Kateryna; Podpletnia, Olena

    2016-01-01

    The study suggests developed potentiometric sensors for determining the concentration of succinic and salicylic acids through using ion associates of succinic acid with safranin T and salicylic acid with safranin T as an electrode­active material of a plasticized film membrane. It is an important task of analytic practice to determine the contents of succinic and salicylic acids in samples with a complex matrix (the environment, foodstuffs, and pharmaceuticals). The research has revealed anal...

  19. Simple Method to Determine the Partition Coefficient of Naphthenic Acid in Oil/Water

    DEFF Research Database (Denmark)

    Bitsch-Larsen, Anders; Andersen, Simon Ivar

    2008-01-01

    The partition coefficient for technical grade naphthenic acid in water/n-decane at 295 K has been determined (K-wo = 2.1 center dot 10(-4)) using a simple experimental technique with large extraction volumes (0.09 m(3) of water). Furthermore, nonequilibrium values at different pH values are prese...

  20. Determination of free fatty acids in cooking oil: traditional spectrophotometry and optothermal window assay

    NARCIS (Netherlands)

    Goyrik, M.; Ajtony, Z.; Doka, O.; Alebic-Juretic, A.; Bicanic, D.D.; Koudijs, A.

    2006-01-01

    The concept of optothermal window (OW) (with 632.8 nm He-Ne laser used as a radiation source), combined with copper soap based colorimetry, was proposed as a new analytical tool to determine total free fatty acid (FFA) content in thermally treated cooking oil. The results obtained were compared to t

  1. Matrix solid-phase dispersion for the liquid chromatographic determination of phenolic acids in Melissa officinalis.

    Science.gov (United States)

    Ziaková, Alica; Brandsteterová, Eva; Blahová, Eva

    2003-01-01

    Matrix solid-phase dispersion (MSPD) was used for sample preparation of plant material (Melissa officinalis, Lemon Balm) prior to liquid chromatography of rosmarinic, caffeic and protocatechuic acids, phenolic compounds present in this herb. Different MSPD sorbents and various elution agents were tested and the optimal extraction conditions determined with the aim to obtain extraction recoveries greater than 90% for all analytes. PMID:12568390

  2. Development of gamma spectrometric method for the determination of thorium in phosphoric acid solution

    Energy Technology Data Exchange (ETDEWEB)

    Mirashi, N.N.; Chaudhury, S.; Aggarwal, S.K. [Fuel Chemistry Div., Bhabha Atomic Research Centre, Mumbai (India)

    2010-07-01

    Gamma spectrometric determination of thorium in sintered thoria dissolved in strong phosphoric acid was studied using a high purity germanium (HPGe) detector. {sup 232}Th was determined using the highly abundant (27%) gamma ray (911.4 keV) emitted by its daughter {sup 228}Ac. The count rates in peak regions were plotted against the amount of thorium present in thorium nitrate working standard solution to obtain a calibration curve and the extent of thoria dissolved in 88% phosphoric acid was determined. Further studies on determination of thorium were carried out using thorium phosphate solutions, instead of using thorium nitrate working standard solutions. The solution of thorium phosphate obtained after quantitative dissolution of thoria in 88% phosphoric acid was also found to give a linear calibration curve at 911.4 keV. Using the calibration curves, expected count rates for thorium in sintered thoria dissolved in 88% phosphoric acid were calculated and were in good agreement ({+-}3%) with the observed count rates. (orig.)

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

  4. Determination of Distribution Coefficient of Nitrous Acid and Evaluation of Influential Factors

    Institute of Scientific and Technical Information of China (English)

    ZHU; Li-yang; CHEN; Yan-xin; TANG; Hong-bin; HE; Hui

    2013-01-01

    Nitrous acid is inevitably present in Purex process,thus,it is desired to build a HNO2 distribution model which could be incorporated into Purex computer simulation code.In this work base titration and diazotization-coupling reaction was used to determine the concentration of HNO3 and HNO2 in both

  5. Determination of solvation and binding site profile within electropolymerised poly(pyrrole-N-propionic acid)

    DEFF Research Database (Denmark)

    Glidle, A.; Swann, M.J.; Gadegaard, Nikolaj;

    2000-01-01

    Specular neutron reflectivity measurements were performed on electropolymerised films of poly(pyrrole-N-propionic acid) to determine the degree to which the solvents are capable of supporting biological macromolecules can penetrate the polymer film. The permeation profile of Ni2+ ions which chelate...

  6. Determination of viral nucleic acids by electrochemical detection array using paramagnetic nanoparticles

    Directory of Open Access Journals (Sweden)

    Dalibor Huska

    2010-12-01

    Full Text Available Simple and express determination of dangerous viruses is one of the most important precautions of their pandemic spreading.Paramegnetic nanoparticles in combination with electrochemicaldetection methods belong to the group of techniques fulfilling these requirements. We were able to isolate and subsequently detect 100 pg/μl of viral nucleic acid by using 1 μl of paramagneticnanoparticles.

  7. Interference of flavonoids with enzymatic assays for the determination of free fatty acid and triglyceride levels

    NARCIS (Netherlands)

    Hoek-van den Hil, E.F.; Beekmann, K.; Keijer, J.; Hollman, P.C.H.; Rietjens, I.; Schothorst, van E.M.

    2012-01-01

    Flavonoids are bioactive food compounds with potential lipid-lowering effects. Commercially available enzymatic assays are widely used to determine free fatty acid (FFA) and triglyceride (TG) levels both in vivo in plasma or serum and in vitro in cell culture medium or cell lysate. However, we have

  8. Amino Acid Profile as a Feasible Tool for Determination of the Authenticity of Fruit Juices

    Directory of Open Access Journals (Sweden)

    Mostafa Asadpoor

    2014-12-01

    Full Text Available Purpose: Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. Methods: The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA. Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the sampled fruit juices. The fruit samples used for this analysis were apples, oranges, cherry, pineapple, mango, apricot, pomegranate, peach and grapes. Results: The results showed that 32% of samples tested in this study had a lower concentrate percentage as compared to that of their labels and/or other possible authenticity problems in the manufacturing process. The following samples showed probable adulteration: four cherry juice samples, two pomegranate juice samples, one mango, three grape, four peach, seven orange, two apple and one apricot juice samples. Conclusion: In general, determining the amount of amino acids and comparing sample amino acids profiles standard values seems to be an indicator for quality control. This method can the regulatory agencies with a tool, to help produce a healthier The aim of this study is the analytical control of the fruit juice composition is becoming an important issue, and HPLC can provide an important and essential tool for more accurate research as well as for routine analysis.

  9. Chemiluminescence of graphene quantum dots and its application to the determination of uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Amjadi, Mohammad, E-mail: amjadi@tabrizu.ac.ir; Manzoori, Jamshid L.; Hallaj, Tooba

    2014-09-15

    We report on the chemiluminescence (CL) of graphene quantum dots (GQDs) induced by direct chemical oxidation. GQDs were prepared by a simple carbonization method and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and Raman spectroscopy. It was found that Ce(IV) could oxidize GQDs to produce a relatively intense CL emission. The mechanism of CL generation was investigated based on the fluorescence and CL emission spectra. It was attributed to the radiative recombination of oxidant-injected holes and thermally excited electrons in the GQDs. In order to show the analytical application potential of GQDs-Ce(IV) CL system, it was applied to the determination of uric acid. Under the optimized conditions, the proposed CL system exhibited excellent analytical performance for determination of uric acid in the range of 1.0×10{sup −6} M–5.0×10{sup −4} M with a limit of detection of 5.0×10{sup −7} M. The method was applied to the determination of uric acid in human plasma and urine samples, with satisfactory results. - Highlights: • Chemiluminescence of graphene quantum dots by direct oxidation was studied. • Intense CL is produced by reaction of graphene quantum dots with Ce(IV). • The new CL system was applied to determination of uric acid in plasma and urine.

  10. Electrochemical Oxidation and Determination of Oxalic Acid at an Exfoliated Graphite-Polystyrene Composite Electrode

    NARCIS (Netherlands)

    Schoonman, J.; Manea, F.; Radovan, C.; Corb, I.; Pop, A.; Burtica, G.; Malchev, P.G.; Picken, S.J.

    2007-01-01

    An exfoliated graphite-polystyrene composite electrode was evaluated as analternative electrode in the oxidation and the determination of oxalic acid in 0.1 M Na2SO4supporting electrolyte. Using CV, LSV, CA procedures, linear dependences I vs. C wereobtained in the concentrations range of oxalic aci

  11. Determination of ascorbic acid in pharmaceutical preparation and fruit juice using modified carbon paste electrode

    Directory of Open Access Journals (Sweden)

    Simona Žabčíková

    2016-06-01

    Full Text Available Acrobic acid is key substance in the human metabolism and the rapid and accurate determination in food is of a great interest. Ascorbic acid is an electroactive compound, however poorly responded on the bare carbon paste electrodes. In this paper, brilliant cresyl blue and multi-walled carbon nanotubes were used for the modification of carbon paste electrode. Brilliant cresyl blue acts as a mediator improving the transition of electrons, whereas multiwalled carbon nanotubes increased the surface of the electrode. Both brilliant cresyl blue and multiwalled carbon nanotubes were added directly to the composite material. The electrochemical behavior of modified electode was determined in electrolyte at various pH, and the effect of the scan rate was also performed. It was shown that the electrochemical process on the surface of the modified carbon paste electrode was diffusion-controlled. The resulted modified carbon paste electrode showed a good electrocatalytic activity towards the oxidation of ascorbic acid at a reduced overpotential of +100 mV descreasing the risk of interferences. A linear response of the ascorbic acid oxidation current measured by the amperometry in the range of 0.1 - 350 µmol.L-1 was obtained applying the sensor for the standard solution. The limit of detection and limit of quantification was found to be 0.05 and 0.15 µmol.L-1, respectively. The novel method was applied for the determination of ascorbic acid in pharmaceutical vitamin preparation and fruit juice, and the results were in good agreement with the standard HPLC method. The presented modification of carbon paste electrode is suitable for the fast, sensitive and very accurate determination of ascorbic acid in fruit juices and pharmaceutical preparation.

  12. Quantitative determination of carboxylic acids, amino acids, carbohydrates, ethanol and hydroxymethylfurfural in honey by (1)H NMR.

    Science.gov (United States)

    del Campo, Gloria; Zuriarrain, Juan; Zuriarrain, Andoni; Berregi, Iñaki

    2016-04-01

    A method using (1)H NMR spectroscopy has been developed to quantify simultaneously thirteen analytes in honeys without previous separation or pre-concentration steps. The method has been successfully applied to determine carboxylic acids (acetic, formic, lactic, malic and succinic acids), amino acids (alanine, phenylalanine, proline and tyrosine), carbohydrates (α- and β-glucose and fructose), ethanol and hydroxymethylfurfural in eucalyptus, heather, lavender, orange blossom, thyme and rosemary honeys. Quantification was performed by using the area of the signal of each analyte in the honey spectra, together with external standards. The regression analysis of the signal area against concentration plots, used for the calibration of each analyte, indicates a good linearity over the concentration ranges found in honeys, with correlation coefficients higher than 0.985 for the thirteen quantified analytes. The recovery studies give values over the 93.7-105.4% range with relative standard deviations lower than 7.4%. Good precision, with relative standard deviations over the range of 0.78-5.21% is obtained. PMID:26593586

  13. Quantitative determination of carboxylic acids, amino acids, carbohydrates, ethanol and hydroxymethylfurfural in honey by (1)H NMR.

    Science.gov (United States)

    del Campo, Gloria; Zuriarrain, Juan; Zuriarrain, Andoni; Berregi, Iñaki

    2016-04-01

    A method using (1)H NMR spectroscopy has been developed to quantify simultaneously thirteen analytes in honeys without previous separation or pre-concentration steps. The method has been successfully applied to determine carboxylic acids (acetic, formic, lactic, malic and succinic acids), amino acids (alanine, phenylalanine, proline and tyrosine), carbohydrates (α- and β-glucose and fructose), ethanol and hydroxymethylfurfural in eucalyptus, heather, lavender, orange blossom, thyme and rosemary honeys. Quantification was performed by using the area of the signal of each analyte in the honey spectra, together with external standards. The regression analysis of the signal area against concentration plots, used for the calibration of each analyte, indicates a good linearity over the concentration ranges found in honeys, with correlation coefficients higher than 0.985 for the thirteen quantified analytes. The recovery studies give values over the 93.7-105.4% range with relative standard deviations lower than 7.4%. Good precision, with relative standard deviations over the range of 0.78-5.21% is obtained.

  14. Quantitative determination of phases in ZrO{sub 2} (MgO) (Y{sub 2}O{sub 3}) using the Rietveld method; Determinacao quantitativa de fases em ZrO{sub 2} - MgO - Y{sub 2}O{sub 3} utilizando o metodo de Rietveld

    Energy Technology Data Exchange (ETDEWEB)

    Castro, Antonio Carlos de

    2007-07-01

    The key objective of this work is the crystallographic characterization of the zircon co-doped with Yttria and magnesium with the application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon monoclinic, tetragonal, and cubic). Samples of zircon polymorph were obtained from zircon doped with Yttria and magnesium at defined molar concentrations. The zircon polymorph stability during subeutetoid aging at 1350 deg C were investigated to determine ZrO{sub 2} - MgO - Y{sub 2}0{sub 3} phases degradation and to define the solid solutions stability environment. ZrO{sub 2} powders doped with 8 mol por cent of MgO and 1 mol por cent of Y{sub 2}O{sub 3}, and 9 mol por cent of MgO and 0 mol por cent of Y{sub 2}O{sub 3} have been prepared by chemical route using the co-precipitation method. These samples have been calcinate at 550 deg C, sintered at 1500 deg C and characterized by the Rietveld method using the X-ray diffraction data. The variation of the lattice parameter, changes in the phase composition and their microstructures are discussed. The application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon tetragonal and cubic) reveals no formation of tetragonal phase and indicating that the matrix is the cubic phase with low concentration of monoclinic phase.(author)

  15. NF EN 14104. July 2003. Fatty compounds derived products. Fatty acids methylic esters (FAME). Determination of the acid index; NF EN 14104. Juillet 2003. Produits derives des corps gras. Esters methyliques d'acides gras (EMAG). Determination de l'indice d'acide

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2003-07-01

    This European standard describes a titration method for the determination of the acid index of slightly colored fatty acids methylic esters (FAME). This method allows the determination of the acid index over a concentration range comprised between 0.10 mg of KOH/g and 1 mg of KOH/g. (J.S.)

  16. Implementation of a constant load method, for determination of crack growth velocities in MEX-03 system of National Institute of Nuclear Research; Implementacion de un metodo de carga constante, para la determinacion de velocidades de crecimiento de grieta en el sistema MEX-03 del ININ

    Energy Technology Data Exchange (ETDEWEB)

    Diaz S, A.; Fuentes C, P.; Merino C, F. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico)], e-mail: angeles.diaz@inin.gob.mx

    2009-10-15

    Whit the objective of to complete the existent techniques for susceptibility evaluation to phenomenon of stress corrosion cracking in laboratories of Applied Sciences Area of National Institute of Nuclear Research; was realized and documented the modification of a high pressure and temperature equipment, identified as MEX-03 to carry out the implementation of a growth and crack propagation assay, using a constant load method. The assay was realized to a specimen of stainless steel AISI 304l type CT of an inch, which was previously thermally sensitize, simulating the typical degradation of this materials type below operation conditions in a BWR. The MEX-03 system, consist from an annexed auto key to a load system which originally was controlled by displacement; therefore were carried out modifications to achieve the control by load. The realized adjustments allowed to maintain a constant load during all the experiment, and as much the temperature conditions (T = 288 C) as of pressure (P = 8 Mpa) were controlled during the assay realization. The steel was exposed to a conditioned ambient with hydrogen gas addition; simulating a well-known alternative chemistry as hydrogen water chemistry that is used to mitigate the phenomenon of stress corrosion cracking, main degradation mechanism of austenitic stainless steels. The continuation of the crack behavior was realized by means of electric potential fall technique and later was validated of visual form through the fractographic analysis of cracked surface. The modification and control of equipment for realization of this experiment is necessary, for what should be carried out new assays, whose results will allow to establish the effect of dynamic and static methods in velocity determination of crack growth to laboratory level; to be considered in the existent models of crack propagation in systems and components in operation. (Author)

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

    International Nuclear Information System (INIS)

    Graphical abstract: Schematic drawing of electrochemical oxidize AA, DA and UA on graphitic carbon nitride nanosheets-graphene oxide composite modified electrode. - Highlights: • Synthesize g-C3N4, GO and CNNS-GO composite. • CNNS-GO composite was the first time for simultaneous determination of AA, DA and UA. • CNNS-GO/GCE displays fantastic selectivity and sensitivity for AA, DA and UA. • CNNS-GO/GCE was applied to detect real sample with satisfactory results. - Abstract: Graphitic carbon nitride nanosheets with a graphite-like structure have strong covalent bonds between carbon and nitride atoms, and nitrogen atoms in the carbon architecture can accelerate the electron transfer and enhance electrical properties effectually. The graphitic carbon nitride nanosheets-graphene oxide composite was synthesized. And the electrochemical performance of the composite was investigated by cyclic voltammetry and differential pulse voltammetry ulteriorly. Due to the synergistic effects of layer-by-layer structures by π-π stacking or charge-transfer interactions, graphitic carbon nitride nanosheets-graphene oxide composite can improved conductivity, electro-catalytic and selective oxidation performance. The proposed graphitic carbon nitride nanosheets-graphene oxide composite modified electrode was employed for simultaneous determination of ascorbic acid, dopamine and uric acid in their mixture solution, it exhibited distinguished sensitivity, wide linear range and low detection limit. Moreover, the modified electrode was applied to detect urine and dopamine injection sample, and then the samples were spiked with certain concentration of three substances with satisfactory recovery results

  18. Simultaneous determination of the concentrations of isoproterenol, uric acid, and folic acid in solution using a novel nanostructurebased electrochemical sensor

    Institute of Scientific and Technical Information of China (English)

    Mohammad Mazloum-Ardakani; Fariba Sabaghian; Alireza Khoshroo; Hossein Naeimi

    2014-01-01

    A carbon paste electrode modified with 2-((7-(2,5- dihydrobenzylideneamino)heptylimino)methyl) benzene-1,4-diol (DHB) and carbon nanotubes were used to simultaneously determine the concen-trations of isoproterenol (IP), uric acid (UA), and folic acid (FA) in solution. First, cyclic voltammetry was used to investigate the redox properties of the modified electrode at various scan rates. Next, the mediated oxidation of IP at the modified electrode is described. At the optimum pH of 7.0, the oxidation of IP occurs at a potential about 90 mV less than that of an unmodified carbon paste elec-trode. Based on the results of differential pulse voltammetry (DPV), the oxidation of IP showed a dynamic range between 10 and 6000 μmol/L, and a detection limit of 1.24 µmol/L. Finally, DPV was used to simultaneously determine the concentrations of IP, UA, and FA in solution at the modified electrode.

  19. Development of procedures for determining the amino acid requirements of chickens by the indicator amino acid oxidation method.

    Science.gov (United States)

    Ewing, H P; Pesti, G M; Bakalli, R I

    2001-02-01

    To better understand the amino acid requirements of chickens, a method is needed to determine a point estimate of the requirement. A method developed to determine the amino acid requirements of piglets and human infants by using the oxidation rate of an indicator amino acid as the test parameter was adapted for use in growing chickens. Polycarbonate chambers measuring 30 x 40 x 30 (L x W x H) were constructed to house one small mature chicken or several small immature chickens and to trap exhaled CO2. In the first experiment, 10-d-old chicks (250 to 300 g each) were feed deprived for 12 h and given 1 g of a methionine-deficient diet (gavage) with L-[1-C14]phenylalanine. Peak oxidation of L-[1-C14]phenylalanine occurred between 30 and 90 min (-200 dpm/g). A linear rate of oxidation (slope = -1.84; r2 = 0.96) was achieved by 120 min after feeding until after 180 min, when oxidation stabilized at a low rate. The second experiment tested different chambers and chicks with the same treatment to show repeatability. There were four chicks (250 to 300 g each) in each of three apparently identical chambers. Chicks were given two meals labeled with L-[1-C14]phenylalanine, 2 h apart. The CV for the 0- and 30-min collections were 17 and 10%, respectively. The CV for the remaining collections remained at <4%. These data supported a system of two feedings, 2 h apart to reduce variability and a collection period that included up to 3 h after the second feeding.

  20. EXTRACTION, QUANTIFICATION, AND MOLAR MASS DETERMINATION OF HYALURONIC ACID EXTRACTED FROM CHICKEN CREST

    Directory of Open Access Journals (Sweden)

    C. S. ROSA

    2008-11-01

    Full Text Available

    Hyaluronic acid (HA is part of the connective tissue. The polymer is composed of alternating units of ß-d-glucuronic acid and N-acetyl-ß-d-glucosamine linked, respectively, via 1-3 and 1-4 bonds. The chicken crest is one of the richest tissues in this polysaccharide. Since Brazil is one of the main chicken exporters in the world, the utilization of the crests of abated animals for the HA obtaining is particularly attractive. The present work sought to extract HA from chicken crest and to determine the molar mass of the extracted acid. Extraction was accomplished by proteolytic digestion with papain during 24 h at 60oC, followed by precipitation with cetylpyridinium chloride (CPC. Hexuronic acid content was determined via the carbazole method, the intrinsic viscosity was measured using the ball viscosimeter, and the molar mass was calculated by extrapolating the calibration line to zero. In addition, qualitative infrared spectroscopy was carried out on the sample using the Bomem MB spectrophotometer. The results show that the extraction method was effective: the extracted acid possesses a large molecular mass, and the extract contains a signifi cant amount of HA.

  1. Determination of caffeic acid in root and rhizome of Black cohosh (Cimicifuga racemosa (L. Nutt.

    Directory of Open Access Journals (Sweden)

    Zapala Karolina

    2014-06-01

    Full Text Available Cimicifuga racemosa, is a plant with a diverse and long history of medicinal use. Caffeic acid, bioactive compound, which often occurs with other polyphenols can influence the biological activity of this plant. The aim of our work was quantitative analysis of caffeic acid in roots and rhizomes of two varieties of C. racemosa. Analysis was performed by HPLC method. The extracts were separated on C18 reversed-phase column using mixture of methanol, water and formic acid (25:75:0.5 v/v/v as a mobile phase. The flow rate of eluent was 1.0 ml·min-1. The obtained validation parameters such as linearity, linear regression equation and precision expressed as a relative standard deviation were adequate for quantitative determination. Caffeic acid was found in all tested extracts. The highest total amount of caffeic acid was determined in C. racemosa var. racemosa (255.3 μg·g-1 while its concentration in C. racemosa var. cordifolia was significantly lower (213.0 μg·g-1.

  2. [Simultaneous determination of pantothenic acid and D-panthenol in cosmetics by high performance liquid chromatography].

    Science.gov (United States)

    Mao, Xiqin; Hu, Xia; Pan, Wei

    2010-11-01

    A high performance liquid chromatographic method (HPLC) and sample pretreatment method were developed for the simultaneous determination of pantothenic acid (vitamin B5) and D-panthenol (provitamin B5) in cosmetics with different matrices (including of creams, lotions, aqueous cosmetics, oily cosmetics, wax-based cosmetics, nail polish etc). A liquid-liquid extraction system composed of water and water-immiscible solvent was used to preliminarily separate the target components from other oil-soluble components and surfactants in cosmetics, then macromolecular water-soluble matrices in cosmetics were removed by coprecipitation with potassium ferrocyanide-zinc acetate precipitating agent, and then under acid condition, pantothenic acid and D-panthenol were enriched on a C18 solid-phase extraction sorbent. After the removal of other water-soluble impurities, target components were eluted by 40% methanol and then separated and quantitatively analyzed by high performance liquid chromatography with external standard method. Good linear relationship was achieved in the concentration range of 0.1-10 microg/g for pantothenic acid and D-panthenol. The linear correlation coefficients were separately 0.998 9 and 0.999 6. The average recoveries of the target components in cosmetics were more than 90%. Limit of detection of the method was 30 microg/g and the limit of quantification was 100 microg/g. This method can be used to simultaneously determine pantothenic acid and D-panthenol in cosmetics. The results are accurate and reliable. PMID:21381423

  3. A method for determining an indicator of effective dose calculation due to inhalation of Radon and its progeny from in vivo measurements; Um metodo para determinar um indicador para calcular dose efetiva devida a inalacao de Radonio e seus descendentes utilizando medicoes in vivo

    Energy Technology Data Exchange (ETDEWEB)

    Estrada, Julio Jose da Silva

    1994-07-01

    Direct measurement of the absolved dose to lung tissue from inhalation of radon and its progeny is not possible and must be calculated using dosimetric models, taking into consideration the several parameters upon which the dose calculation depends. To asses the dose due to inhalation of radon and its progeny, it is necessary to estimate the cumulative exposure. Historically, this has been done using WLM values estimated with measurements of radon concentration in air. The radon concentration in air varies significantly, however, in space with time, and the exposed individual is also constantly moving around. This makes it almost impossible to obtain a precise estimate of an individual's inhalation exposure. This work describes a pilot study to calculate lung dose from the deposition of radon progeny, via estimates of cumulative exposure derived from in vivo measurements of {sup 210} Pb, in subjects exposed to above-average radon and its progeny concentrations in their home environments. The measurements were performed in a whole body counter. With this technique, the exposed individuals become, in affect, their own samplers and dosimeters and the estimate of cumulative exposure is not affected by the variation of the atmospheric concentration of radon and its progeny in time and space. Forty individuals identified as living in homes with radon levels ranging from about 740 Bq/m{sup 3} to 150.000 Bq/m{sup 3} were measured. Also, additional 34 measurements were made on personnel from NYUMC/NIEM who live in a residential area surrounding the laboratory in which the levels of radon have been shown to be at below average values. To realize these measurements a methodology was developed to determine the subject's background, using a head phantom made with a cubic plastic container containing known amounts of potassium and calcium dissolved in four liters of water. The effective doses calculated from the in vivo measurements are compared to effective doses

  4. Direct determination of fatty acids in fish tissues: quantifying top predator trophic connections.

    Science.gov (United States)

    Parrish, Christopher C; Nichols, Peter D; Pethybridge, Heidi; Young, Jock W

    2015-01-01

    Fatty acids are a valuable tool in ecological studies because of the large number of unique structures synthesized. They provide versatile signatures that are being increasingly employed to delineate the transfer of dietary material through marine and terrestrial food webs. The standard procedure for determining fatty acids generally involves lipid extraction followed by methanolysis to produce methyl esters for analysis by gas chromatography. By directly transmethylating ~50 mg wet samples and adding an internal standard it was possible to greatly simplify the analytical methodology to enable rapid throughput of 20-40 fish tissue fatty acid analyses a day including instrumental analysis. This method was verified against the more traditional lipid methods using albacore tuna and great white shark muscle and liver samples, and it was shown to provide an estimate of sample dry mass, total lipid content, and a condition index. When large fatty acid data sets are generated in this way, multidimensional scaling, analysis of similarities, and similarity of percentages analysis can be used to define trophic connections among samples and to quantify them. These routines were used on albacore and skipjack tuna fatty acid data obtained by direct methylation coupled with literature values for krill. There were clear differences in fatty acid profiles among the species as well as spatial differences among albacore tuna sampled from different locations. PMID:25376156

  5. Micellar LC Separation of Sesquiterpenic Acids and Their Determination in Valeriana officinalis L. Root and Extracts

    Directory of Open Access Journals (Sweden)

    Artem U. Kulikov

    2012-01-01

    Full Text Available A simple micellar liquid chromatography (MLC method was developed and validated according to ICH Guidelines for the determination of sesquiterpenic acids (valerenic, hydroxyvalerenic, and acetoxyvalerenic acids in root and rhizome extract from Valeriana officinalis L. and valerian dry hydroalcoholic extract. Samples were analyzed on Nucleosil C18 column (150mm×4.6mm, 5 μm using an isocratic mobile phase which consisted of Brij 35 (5% (w/v aqueous solution; pH 2.3±0.1 by phosphoric acid and 1-butanol (6% (v/v; UV detection was at 220 nm. Micellar mobile phase using allows to fully separate valerenic acids within 25 minutes. Linearity for hydroxyvalerenic, acetoxyvalerenic, and valerenic acids was 1.9–27.9, 4.2–63.0, and 6.1–91·3 μg.mL−1, and limit of detection was 0.14, 0.037, and 0.09 μg·mL−1, respectively. Intraday and interday precisions were not less than 2% for all investigated compounds. The proposed method was found to be reproducible and convenient for quantitative analysis of sesquiterpenic acids in valerian root and related preparations.

  6. GC determination of fatty acids in green beans grown in Galicia (N.W. Spain

    Directory of Open Access Journals (Sweden)

    López Hernández, J.

    1996-06-01

    Full Text Available The concentrations of lauric, myristic, palmitic, palmitoleic, stearic, oleic, linoleic, linolenic, arachidic acids in green beans (Phaseolus vulgaris L. grown in Galicia (N.W. Spain were determinated by capillary gas chromatography (GC. Palmitic acid was the most abundant fatty acid component (113 mg/100 g. of lyophilizate; 35.2% of total fatty acid content, followed by linolenic acid (23.1% and linoleic acid (21.6%.

    Se determinaron, mediante cromatografía gaseosa, las concentraciones de ácidos láurico, mirístico, palmítico, palmitoleico, esteárico, oieico, linoleico, linolénico y araquídico en judías verdes producidas en Galicia (N.O. España. El ácido palmítico fue el más abundante (113 mg/100 g. de liofilizado; 35,2% del contenido total de ácidos grasos, seguido por los ácidos linolénico (23,1% y linoleico (21,6%.

  7. Fast techniques for the evaluation of reservoirs capacity; Metodos de evaluacion rapida de capacidad de yacimentos

    Energy Technology Data Exchange (ETDEWEB)

    Flores Armenta, Magaly del Carmen [Gerencia de Proyectos Geotermoelectricos de la Comision Federal de Electricidad, Morelia (Mexico)

    1995-05-01

    Fast techniques for the evaluation of geothermal reservoirs allow us to have an approach of its electrical potential. Based on the laws of conservation of mass and energy, considering infinite permeability, this paper presents techniques for fast reservoir evaluation. These techniques let us calculate in a very practical way, the electric power that can be obtained from a geothermal field. These techniques can be an important tool to solve practical problems, and are useful during the preliminary development of geothermal sources. [Espanol] Los metodos de evaluacion rapida de yacimientos permiten estimar de manera aproximada la potencia electrica maxima y minima de los mismos. Se presentan tecnicas de evaluacion basadas en las leyes de conservacion de masa y energia, considerando permeabilidad infinita. Las tecnicas utilizadas pueden ser una herramienta importante para la solucion de problemas practicos y para la toma de decisiones en etapas de prefactibilidad.

  8. Chromatographic method for determination of the free amino acid content of chamomile flowers

    Directory of Open Access Journals (Sweden)

    Xiaoli Ma

    2015-01-01

    Full Text Available Objective: To determine the free amino acid contents of chamomile flowers using reverse-phase high-performance column chromatography preceded by pre-column derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC, and to determine the reliability of this method. Materials and Methods: Derivatization with reconstituted AQC was used to prepare the samples and standards for injection into the chromatography column. The peaks were analyzed by fluorescence detection (λ excitation, 250 nm; λ emission, 395 nm. Results: Alanine, proline, and leucine were the most abundant amino acids, whereas tyrosine and methionine were the least abundant. The linearity of the method was found to be good with amino acid concentrations of 0.012-0.36 μM. The precision was 0.05-1.36%; average recovery, 91.12-129.41%; and limit of detection, 0.006-0.058 μM. Conclusion: The method is reliable for determining the free amino acid content of different types of chamomile flowers.

  9. Melamine and Cyanuric Acid do not interfere with Bradford and Ninhydrin assays for protein determination

    OpenAIRE

    Field, Anjalie; Field, Jeffrey

    2010-01-01

    In the fall of 2007 pet food contaminated with melamine and cyanuric acid caused kidney stones in thousands of animals. In the summer of 2008, a more serious outbreak of adulterated dairy food caused the deaths of six infants and sickened about 290,000 children in China. In all cases, melamine was likely added to inflate the apparent protein content of the foods. To determine if we could measure protein without interference from melamine and cyanuric acid we tested these compounds in the Brad...

  10. Determination of abscisic acid based on the fluorescent quenching of quantum dots

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    The quenching mechanism of the fluorescence of quantum dots by abscisic acid has been systematically investigated.The quenching constant KSV = 5.1 × 1011 / M was obtained under the optimized condition.On the basis of that,a very sensitive method for the determination of abscisic acid has been developed.The linear equation was F0/F = 0.9309 + 0.5072 C(pmol/L) and its linear range was 0.2-3.0 pmol/L with a correlation coefficient of 0.9939.The limit of detection was 0.09 pmol/L.

  11. Spectrophotometric determination of thioctic (a-Aipoic acid in water and pharmaceutical preparations

    Directory of Open Access Journals (Sweden)

    ZAGORKA KORICANAC

    2007-01-01

    Full Text Available A spectrophotometric method is described for the assay of thioctic acid. The method is based on the reaction between the drug and palladium(II chloride. In this reaction, a yellow-coloured, water soluble product with a 1:1 stoichiometric ratio and an absorption maximum at 365 nm was formed. The stability of the formed complex depends on various factors (pH, reaction time, concentration of reagents, ionic strength. Based on these findings, a new method is suggested for the spectrophotometric determination of thioctic acid in pharmaceutical formulations. This method is simple, sensitive and reproducible.

  12. Fast mass spectrometry-based enantiomeric excess determination of proteinogenic amino acids.

    Science.gov (United States)

    Fleischer, Heidi; Thurow, Kerstin

    2013-03-01

    A rapid determination of the enantiomeric excess of proteinogenic amino acids is of great importance in various fields of chemical and biologic research and industries. Owing to their different biologic effects, enantiomers are interesting research subjects in drug development for the design of new and more efficient pharmaceuticals. Usually, the enantiomeric composition of amino acids is determined by conventional analytical methods such as liquid or gas chromatography or capillary electrophoresis. These analytical techniques do not fulfill the requirements of high-throughput screening due to their relative long analysis times. The method presented allows a fast analysis of chiral amino acids without previous time consuming chromatographic separation. The analytical measurements base on parallel kinetic resolution with pseudoenantiomeric mass tagged auxiliaries and were carried out by mass spectrometry with electrospray ionization. All 19 chiral proteinogenic amino acids were tested and Pro, Ser, Trp, His, and Glu were selected as model substrates for verification measurements. The enantiomeric excesses of amino acids with non-polar and aliphatic side chains as well as Trp and Phe (aromatic side chains) were determined with maximum deviations of the expected value less than or equal to 10ee%. Ser, Cys, His, Glu, and Asp were determined with deviations lower or equal to 14ee% and the enantiomeric excess of Tyr were calculated with 17ee% deviation. The total screening process is fully automated from the sample pretreatment to the data processing. The method presented enables fast measurement times about 1.38 min per sample and is applicable in the scope of high-throughput screenings.

  13. Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode

    International Nuclear Information System (INIS)

    In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1 M phosphate buffer solution (PBS) at pH 7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 μM over the linear dynamic range of 1.6 μM to 16 μM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples. - Highlights: • Electropolymerization of spands reagent was fabricated by cyclic voltammetry • The Poly (spands reagent) electrode shows excellent electrocatalytic activity for the detection of dopamine. • The detection limit for dopamine was found to be 0.7 μM. • The proposed method can be applied for DA in injection and human blood serum samples

  14. Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Veera Manohara Reddy, Y.; Prabhakara Rao, V.; Vijaya Bhaskar Reddy, A.; Lavanya, M.; Venu, M.; Lavanya, M.; Madhavi, G., E-mail: gmchem01@gmail.com

    2015-12-01

    In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1 M phosphate buffer solution (PBS) at pH 7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 μM over the linear dynamic range of 1.6 μM to 16 μM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples. - Highlights: • Electropolymerization of spands reagent was fabricated by cyclic voltammetry • The Poly (spands reagent) electrode shows excellent electrocatalytic activity for the detection of dopamine. • The detection limit for dopamine was found to be 0.7 μM. • The proposed method can be applied for DA in injection and human blood serum samples.

  15. Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

    International Nuclear Information System (INIS)

    The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

  16. Determination of uric acid in human urine by ion chromatography with conductivity detector

    Institute of Scientific and Technical Information of China (English)

    Fu Yong Zhao; Zong Hua Wang; Hui Wang; Rui Zhao; Ming Yu Ding

    2011-01-01

    A simple, fast, precise and eco-friendly analytical method for the determination of uric acid (UA) in human urine by ion chromatography (IC) was established. The sample pretreatment was not required, only needed centrifugation and filtration. The separation was carried out on a cation exchange column with 2.0 mmol/L nitric acid as mobile phase at the flow-rate 1.0 mL/min. A non-suppressed conductivity detector was used. The IC analysis time for one run was within 10 min under the optimized IC condition. The detection limits were 0.5 μg/L(S/N = 3) for uric acid. The recovery was 100.1 % while the relative standard deviation (RSD) was 1.8% from 10 measurements.

  17. Electrochemical Oxidation and Determination of Oxalic Acid at an Exfoliated Graphite-Polystyrene Composite Electrode

    Directory of Open Access Journals (Sweden)

    Joop Schoonman

    2007-04-01

    Full Text Available An exfoliated graphite-polystyrene composite electrode was evaluated as analternative electrode in the oxidation and the determination of oxalic acid in 0.1 M Na2SO4supporting electrolyte. Using CV, LSV, CA procedures, linear dependences I vs. C wereobtained in the concentrations range of oxalic acid between 0.5 to 3 mM, with LOD =0.05mM, and recovery degree of 98%, without need of surface renewing between successiveruns. The accuracy of the methods was evaluated as excellent comparing the detection resultswith that obtained using conventional KMnO4 titration method. In addition, the apparentdiffusion coefficient of oxalic acid D was found to be around 2.89 · 10-8 cm2·s-1 by CA andCV.

  18. Morphology-dependent Electrochemical Enhancements of Porous Carbon as Sensitive Determination Platform for Ascorbic Acid, Dopamine and Uric Acid

    Science.gov (United States)

    Cheng, Qin; Ji, Liudi; Wu, Kangbing; Zhang, Weikang

    2016-02-01

    Using starch as the carbon precursor and different-sized ZnO naoparticles as the hard template, a series of porous carbon materials for electrochemical sensing were prepared. Experiments of scanning electron microscopy, transmission electron microscopy and Nitrogen adsorption-desorption isotherms reveal that the particle size of ZnO has big impacts on the porous morphology and surface area of the resulting carbon materials. Through ultrasonic dispersion of porous carbon and subsequent solvent evaporation, different sensing interfaces were constructed on the surface of glassy carbon electrode (GCE). The electrochemical behaviors of ascorbic acid (AA), dopamine (DA) and uric acid (UA) were studied. On the surface of porous carbon materials, the accumulation efficiency and electron transfer ability of AA, DA and UA are improved, and consequently their oxidation signals enhance greatly. Moreover, the interface enhancement effects of porous carbon are also controlled by the particle size of hard template. The constructed porous carbon interface displays strong signal amplification ability and holds great promise in constructing a sensitive platform for the simultaneous determination of AA, DA and UA.

  19. Determination of free fatty acids in pharmaceutical lipids by ¹H NMR and comparison with the classical acid value.

    Science.gov (United States)

    Skiera, Christina; Steliopoulos, Panagiotis; Kuballa, Thomas; Diehl, Bernd; Holzgrabe, Ulrike

    2014-05-01

    Indices like acid value, peroxide value, and saponification value play an important role in quality control and identification of lipids. Requirements on these parameters are given by the monographs of the European pharmacopeia. (1)H NMR spectroscopy provides a fast and simple alternative to these classical approaches. In the present work a new (1)H NMR approach to determine the acid value is described. The method was validated using a statistical approach based on a variance components model. The performance under repeatability and in-house reproducibility conditions was assessed. We applied this (1)H NMR assay to a wide range of different fatty oils. A total of 305 oil and fat samples were examined by both the classical and the NMR method. Except for hard fat, the data obtained by the two methods were in good agreement. The (1)H NMR method was adapted to analyse waxes and oleyloleat. Furthermore, the effect of solvent and in the case of castor oil the effect of the oil matrix on line broadening and chemical shift of the carboxyl group signal are discussed.

  20. Direct determination of amino acids by hydrophilic interaction liquid chromatography with charged aerosol detection.

    Science.gov (United States)

    Socia, Adam; Foley, Joe P

    2016-05-13

    A chromatographic analytical method for the direct determination of amino acids by hydrophilic interaction liquid chromatography (HILIC) was developed. A dual gradient simultaneously varying the pH 3.2 ammonium formate buffer concentration and level of acetonitrile (ACN) in the mobile phase was employed. Using a charged aerosol detector (CAD) and a 2(nd) order regression analysis, the fit of the calibration curve showed R(2) values between 0.9997 and 0.9985 from 1.5mg/mL to 50μg/mL (600ng to 20ng on column). Analyte chromatographic parameters such as the sensitivity of retention to the water fraction in the mobile phase values (mHILIC) were determined as part of method development. A degradation product of glutamine (5-pyrrolidone-2-carboxylic acid; pGlu) was observed and resolved chromatographically with no method modifications. The separation was used to quantitate amino acid content in acid hydrolysates of various protein samples. PMID:27059400

  1. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina B. de [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Oliveira, Bras H. de, E-mail: bho@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica

    2013-01-15

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C{sub 18} column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min-1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 {+-} 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  2. Determination of pantothenic acid, biotin, and vitamin B12 in nutritional products.

    Science.gov (United States)

    Hudson, T S; Subramanian, S; Allen, R J

    1984-01-01

    Until recently, liquid chromatographic (LC) methodology for pantothenic acid, biotin, and B12 (cyanocobalamin) has been only marginally successful. These vitamins are difficult to determine by conventional LC techniques and UV detection at 254 or 280 nm, because either the chromophore is inadequate for detection or interference from co-eluting vitamins is overwhelming. Biotin and B12 are usually present in pharmaceutical products at concentrations 100-1000 times lower than other commonly occurring water-soluble vitamins. Co-extraction of all water-soluble vitamins results in gross interferences, especially in LC when the interfering vitamins co-elute with biotin or B12. In addition, pantothenic acid and biotin are colorless in solution and do not exhibit strong UV absorption above 240 nm. As a result, they must be quantitated either by using a low UV wavelength for detection or by derivatizing the vitamin to obtain an adequate chromophore. A description of procedures for LC determination of pantothenic acid, panthenol, cyanocobalamin, and biotin in pharmaceutical products is presented. Pantothenic acid has been measured by using both a derivatization technique and low UV wavelength detection. Biotin has been quantitated by using low UV wavelength detection. The limitations of these techniques are also discussed. Chromatographic separation of cyanocobalamin is complicated by co-eluting vitamins such as riboflavin. It is detected by using the 546 nm wavelength where riboflavin does not interfere. PMID:6501166

  3. Determination of amino acids in two Polysiphonia species and study of enzymatic hydrolysis method

    Science.gov (United States)

    Zhang, Li-Xin; Fan, Xiao; Wei, Yu-Xi

    2002-09-01

    The total content of the rich amino acids in two common red algae, Polysiphonia urceolata and Polysiphonia japonica growing in the Qingdao seashore were determined. The algae powder was hydrolyzed by 6 mol/L HCl at 110°C for 48 h and determined by amino acid analyzer. The content was 25.35% and 24.16%, respectively, much higher than that of some other species. In addition, a nutritive liquid with abundant amino acids was prepared (by the enzymatic hydrolysis method using Polysiphonia urceolata) as raw material for a kind of health beverage. The dried seaweed was decolored by 0.25% KMnO4 and 0.5% active carbon, then enzymalized. In the selection of enzymalizing condition, the orthogonal experimental design was used. Four factors including kinds of enzyme, quantity of enzyme, temperature and time were studied at 3 levels. According to the orthogonal design results, we can choose an optimal condition: hydrolyzing at 45°C by neutral proteinase (0.25%, w/w) for 2h, adjusting pH to 8.5, then adding trypsin (0.25%, w/w) and hydrolyzing for 2 h. Finally the above solution was alkalized by NaOH and neutralized by casein. After the hydrolyzed liquid was filtered and concentrated, suitable additives were added. The final products contain rich amino acids.

  4. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    International Nuclear Information System (INIS)

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C18 column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min−1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 ± 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  5. Spectrophotometric determination of the acidity constants of calcon in water and mixed water–organic solvents

    Directory of Open Access Journals (Sweden)

    MOHAMMAD MAZLOUM-ARDAKANI

    2009-02-01

    Full Text Available The acid–base properties of calcon (1-(2-hydroxy-1-naphthylazo-2-naphthol-4-sulfonic acid in water and mixed water–organic solvents at 25 °C at an ionic strength of 0.10 M are studied by a multiwavelength spectrophotometric method. The organic solvents used were the amphiprotic (methanol, dipolar aprotic (dimethylsulfoxide, and low basic aprotic (acetonitrile. To evaluate the pH absorbance data, a resolution method based on the combination of soft- and hard-modeling was applied. The acidity constants of all related equilibria were estimated using the whole spectral fitting of the collected data to an established factor analysis model. The data analysis program Datan was applied for determination of the acidity constants. The corresponding pKa values were determined in water and mixed water–organic solvents. Linear relationship between the acidity constants and the mole fraction of the different sol-vents in the mixtures exist. The effect of solvent properties on acid–base behavior is discussed.

  6. Determination of free acid by standard addition method in potassium thiocyanate

    Energy Technology Data Exchange (ETDEWEB)

    Baumann, E W

    1982-06-01

    The free acid content of solutions containing hydrolyzable ions has been determined potentiometrically by a standard addition method. Two increments of acid are added to the sample in 1M potassium thiocyanate solution. The sample concentration is calculated by solution of three simultaneous Nernst equations. The method has been demonstrated for solutions containing Al/sup 3 +/, Cr/sup 3 +/, Fe/sup 3 +/, Hg/sup 2 +/, Ni/sup 2 +/, Th/sup 4 +/, or UO/sub 2//sup 2 +/ with a metal-to-acid ratio of < 2.5. The method is suitable for determination of 10 ..mu..moles acid in 10 mL total volume. The accuracy can be judged from the agreement of the Nernst slopes found in the presence and absence of hydrolyzable ions. The relative standard deviation is < 2.5%. The report includes a survey of experiments with thermometric, pH, and Gran plot titrations in a variety of complexants, from which the method was evolved. Also included is a literature survey of sixty references, a discussion of the basic measurements, and a complete analytical procedure.

  7. Compositional characteristics of commercial yoghurt based on quantitative determination of viable lactic acid bacteria

    Directory of Open Access Journals (Sweden)

    Niketić Gordana B.

    2009-01-01

    Full Text Available Yoghurt quality is particularly difficult to standardize because of the many forms, varieties, manufacturing methods, ingredients and consumer preferences that exist. Since these factors will always play an important role, it is unlikely that a uniform yoghurt quality concept will ever emerge, such as has been developed for other dairy products. There are a number of common denominators, however that have bearing on yoghurt quality. Since a number of producers are recognized within the broad category entitled yoghurt. This situation makes yoghurt an interesting, challenging, but also a confusing area to work in. The present investigation was undertaken to isolate from commercial yoghurt the strains involved in its manufacture and determine the characteristics of Streptococcus thermophilus and Lactobacillus delbrueckii subsp.bulgaricus. This study is concerned with the lactic acid bacteria (L.delbrueckii subsp. bulgaricus and S. thermophilus growth in yoghurt from involving different procedures and with the determination of the number of lactic acid bacteria in dependence of the temperature and acidity in the period of storage. Predominant samples of yoghurt were with 11-107/ml lactic acid lactococci (44.28%.

  8. Determination of low molecular weight organic acids in soil, plants, and water by capillary zone electrophoresis.

    Science.gov (United States)

    Li, Ying-Hui; Huang, Bi-Xia; Shan, Xiao-Quan

    2003-03-01

    Determination of low molecular weight organic acids in soils and plants by capillary zone electrophoresis was accomplished using a phthalate buffer and indirect UV detection mode. The influence of some crucial parameters, such as pH, buffer concentration and surfactant were investigated. A good separation of seven organic acids was achieved within 5 min using an electrolyte containing 15 mmol L(-1) potassium hydrogen phthalate, 0.5 mmol L(-1) myristyltrimethylammonium bromide (MTAB), and 5% methanol (MeOH) (v/v) at pH 5.60, separation voltage -20 kV, and temperature 25 degrees C. The relative standard deviation (n=5) of the method was found to be in range 0.18-0.56% for migration time and 3.2-4.8% for peak area. The limit of detection ranged between 0.5 micro mol L(-1) to 6 micro mol L(-1) at a signal-to-noise ratio of 3. The recovery of standard organic acids added to real samples ranged from 87 to 119%. This method was simple, rapid and reproducible, and could be applied to the simultaneous determination of organic acids in environmental samples. PMID:12664177

  9. Coulometric-potentiometric determination of autoprotolysis constant and relative acidity scale of water

    Directory of Open Access Journals (Sweden)

    Džudović Radmila M.

    2010-01-01

    Full Text Available The autoprotolysis constant and relative acidity scale of water were determined by applying the coulometric-potentiometric method and a hydrogen/palladium (H2/Pd generator anode. In the described procedure for the evaluation of autoprotolysis constant, a strong base generated coulometrically at the platinum cathode in situ in the electrolytic cell, in presence of sodium perchlorate as the supporting electrolyte, is titrated with hydrogen ions obtained by the anodic oxidation of hydrogen dissolved in palladium electrode. The titration was carried out with a glass-SCE electrode pair at 25.0±0.1°C. The value obtained pKw = 13.91 ± 0.06 is in agreement with literature data. The range of acidity scale of water is determined from the difference between the halfneutralization potentials of electrogenerated perchloric acid and that of sodium hydroxide in a sodium perchlorate medium. The halfneutralization potentials were measured using both a glass-SCE and a (H2/Pdind-SCE electrode pairs. A wider range of relative acidity scale of water was obtained with the glass-SCE electrode pair.

  10. DETERMINATION OF AMINO ACIDS IN TWO POLYSIPHONIA SPECIES AND STUDY OF ENZYMATIC HYDROLYSIS METHOD

    Institute of Scientific and Technical Information of China (English)

    张立新; 范晓; 魏玉西

    2002-01-01

    The total content ot the nch amino acids in two common red algae, Potystpnoma urceolata and Polysiphonia japonica growing in the Qingdao seashore were determined. The algae powder was hydrolyzed by 6 mol/L HC1 at 110℃ for 48 h and determined by amino acid analyzer. The content was 25.35% and 24.16% , respectively, much higher than that of some other species. In addition, a nutritive liquid with abundant amino acids was prepared (by the enzymatic hydrolysis method using Polysiphonia urceolata ) as raw material for a kind of health beverage. The dried seaweed was decolored by 0.25% KMnO4 and 0.5% active carbon, then enzymalized. In the selection of enzymalizing condition, the orthogonal experimental design was used. Four factors including kinds of enzyme, quantity of enzyme, temperature and time were studied at 3 levels. According to the orthogonal design results, we can choose an optimal condition: hydrolyzing at 45℃ by neutral proteinase (0.25% , w/w) for 2 h, adjusting pH to 8.5, then adding trypsin (0.25% , w/w) and hydrolyzing for 2 h. Finally the above solution was alkalized by NaOH and neutralized by casein. After the hydrolyzed liquid was filtered and concentrated, suitable additives were added. The final products contain rich amino acids.

  11. Glycosyltransferases A and B: Four Critical Amino Acids Determine Blood Type

    Science.gov (United States)

    Rose, Natisha L.; Palcic, Monica M.; Evans, Stephen V.

    2005-12-01

    Human A, B, and O blood type is determined by the presence or absence of distinct carbohydrate structures on red blood cells. Type O individuals have α-fucose(1→2)galactose disaccharides [O(H) structures] on their cell surfaces while in type A or B individuals, the O antigen is capped by the addition of an α- N -acetylgalactosamine or α-galactose residue, respectively. The addition of these monosaccharides is catalyzed by glycosyltransferase A (GTA) or glycosyltransferase B (GTB). These are homologous enzymes differing by only 4 amino acids out of 354 that change the specificity from GTA to GTB. In this review the chemistry of the blood group ABO system and the role of GTA, GTB, and the four critical amino acids in determining blood group status are discussed. See JCE Featured Molecules .

  12. Determination of essential fatty acids and long chain polyunsaturated fatty acids in complimentary infant foods in the UK

    OpenAIRE

    Loughrill, Emma; Zand, Nazanin

    2014-01-01

    The study reported herein was conducted to establish the concentration of two essential fatty acids; linoleic acid (LA) 18:2 n-6 and α-linolenic acid (ALA) 18:3 n-3; and three long chain poly unsaturated fatty acids (LCPUFA); eicosapentaenoic acid (EPA) 20:5 n-3, decosahexaenoic acid (DHA) 22:6 n-3 and arachidonic acid (AA) 20:4 n-6 in fish based commercial infant foods in the UK. Quantitative analyses were conducted on four different products using charged aerosol detection HPLC. The total ...

  13. Determination of fruit characteristics, fatty acid profile and total antioxidant capacity of Mespilus germanica L. fruit

    OpenAIRE

    Hale Seçilmiş Canbay; Ersin Atay; Serdal Oğüt

    2015-01-01

    Objective: To determine fruit characteristics, fatty acid profile and total antioxidant capacitiy of first cultured Mespilus germanica L. Methods: A total of 15 fruits were taken randomly from four directions of adult trees. Then the physical and chemical properties of first cultured medlar fruit (Istanbul/Turkey) were measured by using refractometer, colorimeter, spectrophotometer and gas chromatograph mass spectrometer, respectivly. Results: In the fruit studied, the resul...

  14. Algerian mint species: high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    OpenAIRE

    Brahmi Fatiha; Madani Khodir; Stévigny Caroline; Chibane Mohamed; Duez Pierre

    2014-01-01

    Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints, Mentha spicata L. (M. spicata), Mentha pulegium L. and Mentha rotundifolia (L.) Huds by high performance thin layer chromatography (HPTLC)-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation. Methods: The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform: acetone: formic acid (75:16.5:8.5, v/v) as the mobile phase....

  15. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

    Science.gov (United States)

    Popov, L

    2016-09-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials.

  16. Electrocatalytic determination of epinephrine and uric acid using a novel hydroquinone modified carbon paste electrode

    Institute of Scientific and Technical Information of China (English)

    Mohammad Mazloum-Ardakani; Zahra Taleat; Hadi Beitollahi; Hossein Naeimi

    2011-01-01

    A sensitive and selective electrochemical method for the determination of epinephrine (EP) was developed using a modified carbon paste electrode (MCPE) with 2,2'- [3,6-dioxa-l,8-octanediylbis(nitriloethylidyne)]-bis-hydroquinone (DOH). Cyclic vol-tammetry was used to investigate the redox properties of this modified electrode at various solution pH values and at various scan rates. In differential pulse voltammetry, the modified electrode could separate the oxidation peak potentials of EP and uric acid (UA) present in the solution but at the unmodified CPE the peak potentials were indistinguishable. This method was also examined for determination of EP in EP injection.

  17. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

    Science.gov (United States)

    Popov, L

    2016-09-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials. PMID:27451111

  18. Total Acid Value Titration of Hydrotreated Biomass Fast Pyrolysis Oil: Determination of Carboxylic Acids and Phenolics with Multiple End-Point Detection

    Energy Technology Data Exchange (ETDEWEB)

    Christensen, E.; Alleman, T. L.; McCormick, R. L.

    2013-01-01

    Total acid value titration has long been used to estimate corrosive potential of petroleum crude oil and fuel oil products. The method commonly used for this measurement, ASTM D664, utilizes KOH in isopropanol as the titrant with potentiometric end point determination by pH sensing electrode and Ag/AgCl reference electrode with LiCl electrolyte. A natural application of the D664 method is titration of pyrolysis-derived bio-oil, which is a candidate for refinery upgrading to produce drop in fuels. Determining the total acid value of pyrolysis derived bio-oil has proven challenging and not necessarily amenable to the methodology employed for petroleum products due to the different nature of acids present. We presented an acid value titration for bio-oil products in our previous publication which also utilizes potentiometry using tetrabutylammonium hydroxide in place of KOH as the titrant and tetraethylammonium bromide in place of LiCl as the reference electrolyte to improve the detection of these types of acids. This method was shown to detect numerous end points in samples of bio-oil that were not detected by D664. These end points were attributed to carboxylic acids and phenolics based on the results of HPLC and GC-MS studies. Additional work has led to refinement of the method and it has been established that both carboxylic acids and phenolics can be determined accurately. Use of pH buffer calibration to determine half-neutralization potentials of acids in conjunction with the analysis of model compounds has allowed us to conclude that this titration method is suitable for the determination of total acid value of pyrolysis oil and can be used to differentiate and quantify weak acid species. The measurement of phenolics in bio-oil is subject to a relatively high limit of detection, which may limit the utility of titrimetric methodology for characterizing the acidic potential of pyrolysis oil and products.

  19. Methods for vanadium determination in fuel oil by GF AAS with microemulsification and acid digestion sampling

    Energy Technology Data Exchange (ETDEWEB)

    Amorim, Fabio Alan C. [Universidade Federal da Bahia (UFBA), Barreiras, BA (Brazil). Instituto de Ciencias Ambientais e Desenvolvimento Sustentavel; Amaro, Joana A.A.; Lima, Daniel C.; Ferreira, Sergio L.C. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica]. E-mail: slcf@ufba.br; Vale, Maria Goreti R. [PETROBRAS, Sao Francisco do Conde, BA (Brazil). Refinaria Landulfo Alves

    2007-07-01

    Two methods for vanadium determination in fuel oil are proposed using GF AAS. The first is based on the preparation of a microemulsion followed by direct injection into the graphite tube. The pyrolysis and atomization temperatures, 1500 and 2700 deg C, respectively, were chosen from the temperature curves. This procedure allows determination of vanadium with a detection limit of 0.10 {mu}g g{sup -1} and characteristic mass of 87 pg. The other method uses total acid digestion of the sample with sulfuric acid, nitric acid and hydrogen peroxide. In this procedure, the pyrolysis and atomization temperatures recommended were 1000 and 2700 deg C, respectively. Among the analytical characteristics for this method are a detection limit of 0.25 {mu}g g{sup -1} and a characteristic mass of 63 pg. The accuracy of both procedures was confirmed by the determination of vanadium in the certified reference material NIST SRM 1634c-trace metals in fuel oil. (author)

  20. Catalytic Kinetic Determination of Micro Amounts of Oxalic Acid by Second-Order Derivative Oscillopolarography

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    It was found that micro amounts of oxalate showed a very strong catalytic effect on the slow reaction between K2Cr2O7 and Orange Ⅳ in a diluted sulfuric acid medium in a water bath at 70 ℃. Orange Ⅳ exhibited a sensitive second-order derivative polarographic wave at -0.50 V(vs. SCE). This provides the basis for a sensitive and selective catalytic kinetic method for oxalate determination with second-order derivative oscillopolarography. The effects of sulphuric acid, K2Cr2O7, and orange Ⅳ concentrations, reaction temperature and reaction time were investigated. A calibration curve of oxalate in the range of 0.1—2.0 μg/mL was obtained by the fixed-time procedure. The detection limit was 0.03 μg/ mL. The possible interference from co-existing substances or ions was examined. The new method has a high sensitivity and a good selectivity compared to other existing methods for oxalic acid determination. It has been applied to the determination of micro amounts of oxalate in real urine samples with satisfactory results.

  1. Luminescent determination of trace amounts of terbium using diantipyrylmethane and salicylic acid

    International Nuclear Information System (INIS)

    To elucidate the possibility of using pyrazolone-5-diantipyril-methane (DAM) derivative for determination of terbium microimpurities, the conditions have been studied of luminescent determination of terbium in complex compounds containing an ion of rare-earth element, diantipyrilmethane, and salicylic acid (Sal.). The ratio between the components in the complex REE-DAM-Sal is 1:1:3. La, Y, Gd do not affect the luminescence intensity of terbium complex. A luminescent method of determining terbium traces in highly pure oxides of lanthanum, gadolinium, lutetium, and yttrium has been developed in which suspensions of complex precipitation are used. The amount of terbium determined in oxide of lanthanum, gadolinium, and lutetium is (1-5)x10-6% and (2-3)x10-5% in yttrium oxide

  2. Sensitive determination of D-amino acids in mammals and the effect of D-amino-acid oxidase activity on their amounts.

    Science.gov (United States)

    Hamase, Kenji; Konno, Ryuichi; Morikawa, Akiko; Zaitsu, Kiyoshi

    2005-09-01

    The determination of small amounts of D-amino acids in mammalian tissues is still a challenging theme in the separation sciences. In this review, various gas-chromatographic and high-performance liquid chromatographic methods are discussed including highly selective and sensitive column-switching procedures. Based on these methods, the distributions of D-aspartic acid, D-serine, D-alanine, D-leucine and D-proline have been clarified in the mouse brain. As the regulation mechanisms of D-amino acid amounts in mammals, we focused on the D-amino-acid oxidase, which catalyzes the degradation of D-amino acids. Using the mutant mouse strain lacking D-amino-acid oxidase activity, the effects of the enzymatic activity on the amounts and distributions of various D-amino acids have been investigated. PMID:16141519

  3. Determination of Antioxidant, Anticholinesterase, Tyrosinase Inhibitory Activities and Fatty Acid Profiles of 10 Anatolian Klasea Cass. Species

    Directory of Open Access Journals (Sweden)

    Gülsen Tel

    2015-08-01

    Full Text Available In search of new natural fatty acid sources, extract of 10 different Turkish Klasea species were studies. Fatty acids of Klasea species were studied by GC and GC-MSD. Oleic acid (4.8-45.8%, palmitic acid (15.6-51.8%, linoleic acid (0.3-45.5%, palmitoleic acid (0.8-28.4% and linolenic acid (15.6-34.6% were the main fatty acids elucidated. All extracts were also subjected to acetylcholinesterase, butyrylcholinesterase, tyrosinase, β-carotene-linoleic acid, DPPH • scavenging, CUPRAC and ferrous ion-chelating ability activities. Total flavonoid and phenolic contents were determined as quercetin and pyrocatechol equivalents. All extracts showed significant antioxidant activity in all tests, except hexane extracts of K. serratuloides and K. cerinthifolia that showed weak inhibition against BChE and AChE. The hexane extract of K. coriaceae and methanol extract of K. serratuloides exhibited notable tyrosinase inhibitory activity.

  4. Weak Acid Ionization Constants and the Determination of Weak Acid-Weak Base Reaction Equilibrium Constants in the General Chemistry Laboratory

    Science.gov (United States)

    Nyasulu, Frazier; McMills, Lauren; Barlag, Rebecca

    2013-01-01

    A laboratory to determine the equilibrium constants of weak acid negative weak base reactions is described. The equilibrium constants of component reactions when multiplied together equal the numerical value of the equilibrium constant of the summative reaction. The component reactions are weak acid ionization reactions, weak base hydrolysis…

  5. O-Anisidine as Indicator in Titrimetric Determination of Ascorbic Acid and Isonicotinic Acid Hydrazide in Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    B.S.A.Andrews

    2010-10-01

    Full Text Available Inspite of the beautiful red coloured oxidized product of O-anisidine, the studies on its application in analytical techniques are scanty. So, authors have taken up the investigation on the utility of O-anisidine as a new Analytical reagent in the bromatometric-Indicator reaction. The detailed reaction on the potassium bromate and OAnisidine has enabled the authors to utilize O-Anisidine in titration of Ascorbic Acid and Isonicitonic Acid Hydrazide. Suitable conditions has been established with different acids viz., hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid to give sharp colour change at the equivalence point. The present method has been applied for the estimation of Ascorbic acid and also Isonicitonic Acid Hydrazide in pharmaceutical formulations and results obtained are in good agreement with the values obtained by standard methods

  6. [Determination of protocatechuic acid in rat plasma by high performance liquid chromatography].

    Science.gov (United States)

    Han, Ying; Xiong, Zhili; Yang, Chunjuan; Liu, Man; Li, Famei

    2007-03-01

    A method was developed for the quantitative determination of protocatechuic acid in rat plasma by high performance liquid chromatography (HPLC). With added p-hydroxybenzoic acid as internal standard, the plasma samples were extracted with a solvent mixture of methanol and acetonitrile ( 1: 5, v/v). The analyte was determined by HPLC with a Diamondsil C18 column and a mobile phase of acetonitrile-water (adjusted to pH 2.5 with H3PO4, 9: 91, v/v) at a flow rate of 1. 2 mL/min. The UV detection wavelength was 260 nm. The assay exhibited a good linearity in the concentration range from 0. 050 to 3. 20 mg/L with a correlation coefficient of 0. 997 8. The limit of quantification was 0. 050 mg/L. The relative standard deviations of intra-day and inter-day determination were both less than 7. 0% and the accuracy ranged from - 1. 4% to 2. 6%. The extraction recoveries of protocatechuic acid from rat plasma samples at three concentration levels were 83. 4%, 87. 3%, and 91. 1%, respectively. The developed method was applied to a pharmacokinetic study. The main pharmacokinetic parameters in rats after a single oral dose of 10 mL/kg body weight were as follows: Cmax of (3. 16 +0. 03) microg/mL, tmax of (0. 50 +/- 0. 00) h, AU0-->t of (39. 9 +/- 5. 9) microg x mL(-1) x h, AUC-->infinity of (54. 8 +/- 8. 1) microg x mL(-1) x h and t1/2 of (3. 87 +/- 0. 25) h. The method was proved to be simple, sensitive and accurate, thus suitable for the pharmacokinetic study of protocatechuic acid in rat plasma. PMID:17580687

  7. Simultaneous separation and quantitative determination of monosaccharides, uronic acids, and aldonic acids by high performance anion-exchange chromatography coupled with pulsed amperometric detection in corn stover prehydrolysates

    Directory of Open Access Journals (Sweden)

    Xing Wang

    2012-11-01

    Full Text Available A method for simultaneous separation and quantitative determination of arabinose, galactose, glucose, xylose, xylonic acid, gluconic acid, galacturonic acid, and glucuronic acid was developed by using high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD. The separation was performed on a CarboPacTM PA-10 column (250 mm × 2 mm with a various gradient elution of NaOH-NaOAc solution as the mobile phase. The calibration curves showed good linearity (R2 ≥ 0.9993 for the monosaccharides, uronic acids, and aldonic acids in the range of 0.1 to 12.5 mg/L. The detection limits (LODs and the quantification limits (LOQs were 4.91 to 18.75 μg/L and 16.36 to 62.50 μg/L, respectively. Relative standard deviations (RSDs of the retention times and peak areas for the seven consecutive determinations of an unknown amount of mixture were 0.15% to 0.44% and 0.22% to 2.31%, respectively. The established method was used to separate and determine four monosaccharides, two uronic acids, and two aldonic acids in the prehydrolysate from dilute acid steam-exploded corn stover within 21 min. The spiked recoveries of monosaccharides, uronic acids, and aldonic acids ranged from 91.25% to 108.81%, with RSDs (n=3 of 0.04% ~ 6.07%. This method was applied to evaluate the quantitative variation of sugar and sugar acid content in biomass prehydrolysates.

  8. Fluorescence Quenching Investigation for Janus Green B and used as Probe in Determination of Nucleic Acids

    Institute of Scientific and Technical Information of China (English)

    陈莉华; 刘六战; 沈含熙

    2005-01-01

    Fluorescence quenching of janus green B (JGB) in sodium dodecyl sulfate (SDS) micelle by nucleic acids (DNA) was studied using UV-vis absorption, steady state fluorescence emission methods and lifetime measurements. In the SDS micelle, weak fluorescence of JGB was enhanced, and the maximum emission shifted from 425 to 410 nm. In the presence of DNA, the fluorescence of JGB was quenched. Linear relationships between the fluorescence quenching (F0/F) and concentrations of DNA were observed in the range of 2.4×10-8 to 1.08×10-7mol·L-1 for calf thymus nucleic acids (ct DNA) and 1.9×10-8 to 3.8×10-8 mol·L-1 for fish sperm nucleic acids (fs DNA) when 2.5×10-5 mol·L-1 JGB was employed. The limit detection were 1.3×10-8 mol·L-1 for ct DNA and 6.4×10-9 mol·L-1 for fs DNA. At high DNA concentration, there was a systematic deviation from the Stem-Volmer equation due to the static and dynamic quenching occurring simultaneously. The proposed method was applied to the determination of the nucleic acids in chicken blood extraction and the analytical results were in good agreement with the UV-method.

  9. Determination of dissociation parameters of weak acids in different media according to the isohydric method.

    Science.gov (United States)

    Michałowski, Tadeusz; Pilarski, Bogusław; Asuero, Agustin G; Dobkowska, Agnieszka; Wybraniec, Sławomir

    2011-10-30

    The isohydricity (pH constancy) principle is referred to the pair of solutions: weak acid (HL, C(0)mol/L) and strong acid (HB, C mol/L) when mixed e.g., according to titrimetric mode. Such a case takes place if the relation C(0)=C+C(2) × 10(pK(1)) is valid, where pK(1)=-log K(1), K(1) - dissociation constant for a weak monoprotic acid HL. This principle, outlined and formulated in earlier paper (Michałowski et al., Talanta 82 (2010) 1965), is the basis for a sensitive method of pK(1) determination, confirmed for a series of weak acids in presence of basal electrolytes or in water+organic solvent (dimethyl sulphoxide, methanol, isopropanol) media. The results of titrations were elaborated according to principles of regression analysis, with use of least squares method. A new criterion for precision of the results obtained according to this method is formulated. The pK(1) values obtained are comparable with ones found in literature.

  10. Method for determination of fatty acids in bovine colostrum using GC-FID.

    Science.gov (United States)

    Yurchenko, S; Sats, A; Poikalainen, V; Karus, A

    2016-12-01

    Bovine colostrum is potentially valuable source of essential fatty acids (FAs), but so far only few studies have made the effort to estimate FA composition of this potential resource. The aim of current research was to fill this gap with selecting and validating an accurate procedure for the analysis of the composition of the FAs in bovine colostrum. We used colostrum samples of Holstein-Friesian cattle from Märja experimental farm as a test material. The validated method includes derivatization, in which FAs are sent through esterification with the acidic catalyst boron trifluoride. Formed methyl esters of fatty acids (FAMEs) were analysed using GC-FID. The obtained LOD and the LOQ of FAMEs were 0.11-0.68 and 0.37-2.27ppm, respectively. The analysis of fortified samples showed very good and similar recoveries, indicating that the method proposed here can be routinely used for determination and investigation of the fatty acids in dairy products. PMID:27374514

  11. The determination of titratable acidity and total tannins in red wine

    Directory of Open Access Journals (Sweden)

    Rajković Miloš B.

    2009-01-01

    Full Text Available Titration acidity and content of total tannins in mass-market red wines are analyzed in this paper. The content of total acids in wine, expressed through wine acid, was analyzed by potentiometric titration on 7.00 pH value. According to titratable acidity in analyzed wines, all wines (only with analyzed parameters according to Regulations about wine quality. The analysis of differential potentiometric curves shows that these curves can give the answer to the question if non organic substances, amino groups and phenols are present in wine in large quantity, as they are always present in wine. However it doesn't give the clear answer which substances are present in analyzed samples. The answer to this question can be received only by the method of ionic chromatography. The content of total tannins shows short time of storage in wine cellars so wine wasn't stored long enough, i.e. they are commercial wines made for mass market production and consumption. Although they have less content of total tannin materials of given values, wine taste gives the correlation with other polyphenol materials that only give odour, aroma and 'bouquet' to wine. The relative error of mean value is very low which indicates the reproduction of results and reliability of the method of determination of total tannins in red wine.

  12. Determining surface areas of marine alga cells by acid-base titration method.

    Science.gov (United States)

    Wang, X; Ma, Y; Su, Y

    1997-09-01

    A new method for determining the surface area of living marine alga cells was described. The method uses acid-base titration to measure the surface acid/base amount on the surface of alga cells and uses the BET (Brunauer, Emmett, and Teller) equation to estimate the maximum surface acid/base amount, assuming that hydrous cell walls have carbohydrates or other structural compounds which can behave like surface Brönsted acid-base sites due to coordination of environmental H2O molecules. The method was applied to 18 diverse alga species (including 7 diatoms, 2 flagellates, 8 green algae and 1 red alga) maintained in seawater cultures. For the species examined, the surface areas of individual cells ranged from 2.8 x 10(-8) m2 for Nannochloropsis oculata to 690 x 10(-8) m2 for Dunaliella viridis, specific surface areas from 1,030 m2.g-1 for Dunaliella salina to 28,900 m2.g-1 for Pyramidomonas sp. Measurement accuracy was 15.2%. Preliminary studies show that the method may be more promising and accurate than light/electron microscopic measurements for coarse estimation of the surface area of living algae. PMID:9297794

  13. High-performance liquid chromatographic determination of linoleic acid peroxide-derived radicals using electrochemical detection.

    Science.gov (United States)

    Iwahashi, H

    2000-12-29

    High-performance liquid chromatography-electrochemical detection (HPLC-ED) was applied to detect 13-hydroperoxide octadecadienoic acid (13-HPODE)-derived radicals such as the pentyl radical and octanoic acid radical. The 13-HPODE-derived radicals were successfully detected using HPLC-ED by the combined use of the spin-trapping technique with alpha-(4-pyridyl-1-oxide)-N-tert-butylnitrone (4-POBN). The 4-POBN-pentyl radical adduct was detected at the retention time of 18.2 +/- 0.3 min on the elution profile of HPLC-ED with an ODS column (15 cm x 4.6 mm I.D.) using a flow-rate of 1.0 ml/min with 50 mM ammonium acetate in 29% (v/v) aqueous acetonitrile. The 4-POBN-octanoic acid radical adduct was also detected at the retention time of 13.7 +/- 0.7 min using a flow-rate of 1.0 ml/min with 50 mM ammonium acetate in 14% (v/v) aqueous acetonitrile. The concentrations of the 4-POBN radical adducts were determined using HPLC-ED without an internal standard. HPLC-ED is 100 times as sensitive as HPLC-electron spin resonance (ESR) under the ESR and ED conditions employed here. Even 1.8 pmol of the 4-POBN-pentyl (or octanoic acid) radical adduct was detectable using PMID:11204234

  14. Determination of acrylamide and acrylic acid by isocratic liquid chromatography with pulsed electrochemical detection.

    Science.gov (United States)

    Casella, Innocenzo G; Pierri, Marianna; Contursi, Michela

    2006-02-24

    The electrochemical behaviour of the polycrystalline platinum electrode towards the oxidation/reduction of short-chain unsaturated aliphatic molecules such as acrylamide and acrylic acid was investigated in acidic solutions. Analytes were separated by reverse phase liquid chromatographic and quantified using a pulsed amperometric detection. A new two-step waveform, is introduced for detection of acrylamide and acrylic acid. Detection limits (LOD) of 20 nM (1. 4 microg/kg) and 45 nM (3.2 microg/kg) were determined in water solutions containing acrylamide and acrylic acid, respectively. Compared to the classical three-step waveform, the proposed two-step waveform shows favourable analytical performance in terms of LOD, linear range, precision and improved long-term reproducibility. The proposed analytical method combined with clean-up procedure accomplished by Carrez clearing reagent and subsequent extraction with a strong cation exchanger cartridges (SPE), was successfully used for the quantification of low concentrations of acrylamide in foodstuffs such as coffee and potato fries. PMID:16426623

  15. Determination of Organic Acids in Root Exudates by High Performance Liquid Chromatography:Ⅱ.Influence of Several Testing COnditions

    Institute of Scientific and Technical Information of China (English)

    SHENJIANBO; ZHANGFUSUO; 等

    1999-01-01

    Effects of column temperature and flow rate on separation of organic acids were studied by determining nine low-molecular-weight organic acids on reversed-phase C18 column using high performace liquid chromatography(HPLC) with a wavelength of UV(ultraviolet)214 nm and a mobile phase of 18 mmol L-1 KH2PO4 buffer solution (pH2.1).The thermal stabiltiy of organic acids was determined by comparing the recoveries of organic acids in different temperature treatments.The relationships between column temperature,flow rate or solvent pH and retention time were analyzed.At low solvent pH,separatioin efficiency of organic acids was increased by raising the flow rate of the solvent because of lowering the retention time or organic acids.High column temperature was unfavorable for the separation of organic acids.The separating effect can be enhanced through reducing column temperature in organic acid determination due to increasing retention time.High thermal stability of organic acids with low concentrations was observed at temperature of 40℃-45℃,Sensitivity and separation effect of organic acid determination by HPLC were clearly improved by a combination of raising flow rate and lowering column temperature at low solvent pH.

  16. Sensitive spectrophotometric determination of ascorbic acid in drugs and foods using surface plasmon resonance band of silver nanoparticles

    Directory of Open Access Journals (Sweden)

    Kobra Zarei

    2015-12-01

    Full Text Available A simple and sensitive procedure was proposed for spectrophotometric determination of ascorbic acid. It was found that the reduction of Ag+ to silver nanoparticles (Ag-NPs by ascorbic acid in the presence of polyvinylpyrrolidone (PVP as a stabilizing agent produce very intense surface plasmon resonance peak of Ag-NPs. The plasmon absorbance of the Ag-NPs at λ = 440 nm allows the quantitative spectrophotometric detection of the ascorbic acid. The calibration curve was linear with concentration of ascorbic acid in the range of 0.5–60 μM. The detection limit was obtained as 0.08 μM. The influence of potential interfering substances on the determination of ascorbic acid was studied. The proposed method was successfully applied for the determination of ascorbic acid in some powdered drink mixtures, commercial orange juice, natural orange juice, vitamin C injection, effervescent tablet, and multivitamin tablet.

  17. Fluorometric determination of acid proteinase activity in Candida albicans strains from diabetic patients with vulvovaginal candidiasis.

    Science.gov (United States)

    Yildirim, Zuhal; Kilic, Nedret; Kalkanci, Ayse

    2011-09-01

    Vulvovaginal candidiasis is one of the most frequent disorders in obstetrics and gynaecology. Approximately three-quarters of all adult women experience at least one episode of vulvovaginal candidiasis during their life span. Diabetes mellitus (DM) increases the rate of vaginal colonisation and infection with Candida species. The secreted acid proteinase might be especially relevant in the pathogenesis of vulvovaginal candidiasis. The aim of this study was to determine the acid proteinase activity in the samples of Candida albicans from diabetic patients with vulvovaginal candidiasis by a fluorometric method. Vaginal swabs were taken from 33 women (aged between 22 and 57 years) having symptoms of vaginitis. Patients were divided into three groups: control group, controlled diabetic group and uncontrolled diabetic group. The proteinase activity in the culture supernatants was determined by a modified fluorometric method. Acid proteinase activities were significantly increased in the uncontrolled diabetic group in comparison with both the control group and the controlled diabetic group (P albicans pathogenesis in diabetic patients. Improving glucose control may reduce the risk of Candida colonisation and potentially symptomatic infection, among women with diabetes and hence may be useful even for weaker enzyme activity measurements.

  18. An Exact Method to Determine the Conductivity of Aqueous Solutions in Acid-Base Titrations

    Directory of Open Access Journals (Sweden)

    Norma Rodríguez-Laguna

    2015-01-01

    Full Text Available Several works in the literature show that it is possible to establish the analytic equations to estimate the volume V of a strong base or a strong acid (Vb and Va, resp. being added to a solution of a substance or a mix of substances during an acid-base titration, as well as the equations to estimate the first derivative of the titration plot dpH/dV, and algebraic expressions to determine the buffer β capacity with dilution βdil. This treatment allows establishing the conditions of thermodynamic equilibria for all species within a system containing a mix of species from one or from various polyacid systems. The present work shows that it is possible to determine exactly the electric conductivity of aqueous solutions for these Brønsted acid-base titrations, because the functional relation between this property and the composition of the system in equilibrium is well known; this is achieved using the equivalent conductivity λi values of each of the ions present in a given system. The model employed for the present work confirms the experimental outcomes with the H2SO4, B(OH3, CH3COOH, and H3PO4 aqueous solutions’ titration.

  19. Polymorphisms in the fatty acid desaturase genes and diet are important determinants of infant docosahexaenoic acid status

    DEFF Research Database (Denmark)

    Lauritzen, L.; Harsløf, L.; Larsen, L.H.;

    2013-01-01

    Tissue docosahexaenoic acid (DHA) accretion in early infancy is supported by DHA in breast-milk and may thus decrease once complementary feeding takes over. Endogenous synthesis of DHA from alphalinolenic acid is low and polymorphisms in the genes that encodes the fatty acid desaturases (FADS) has...

  20. Algerian mint species: high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Directory of Open Access Journals (Sweden)

    Brahmi Fatiha

    2014-12-01

    Full Text Available Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints, Mentha spicata L. (M. spicata, Mentha pulegium L. and Mentha rotundifolia (L. Huds by high performance thin layer chromatography (HPTLC-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation. Methods: The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform: acetone: formic acid (75:16.5:8.5, v/v as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method. Results: Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1 000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively. The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox® equivalents as a natural source for inhibitors of lipid peroxidation. Conclusions: Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  1. Algerian mint species:high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Institute of Scientific and Technical Information of China (English)

    Brahmi Fatiha; Madani Khodir; Stvigny Caroline; Chibane Mohamed; Duez Pierre

    2014-01-01

    Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints,Mentha spicata L. (M. spicata), Mentha pulegium L. and Mentha rotundifolia (L.) Huds by high performance thin layer chromatography (HPTLC)-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation.Methods:The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform:acetone: formic acid (75:16.5:8.5, v/v) as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method.Results:Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively). The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox®equivalents) as a natural source for inhibitors of lipid peroxidation.Conclusions:Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  2. Studies on the structure of peat humic acid (II). Study on the determination of the aromatic skeletons in peat humic acid by zinc-dust distillation

    Energy Technology Data Exchange (ETDEWEB)

    Oka, H.; Sasaki, M.

    1979-01-01

    In order to determine aromatic skeletons in the chemical structure of peat humic acid, zinc-dust distillation was carried out at 500 C for 2 hours in a stream of hydrogen, and the results compared to those from other substances such as phtholic acid, cumarin, naphthoquinone and ..cap alpha..-lactone. Subsequently, methods for the identification and semi-quantitative determination of polycyclic aromatic hydrocarbons were applied. The total yield of polycyclic hydrocarbon having anthracene, pyrene and perylene rings was 1.9% of the original peat humic acid. However, the yield of aromatic hydrocarbons containing 3 to 5 rings from peat humic acid was approximately equal to those from the other substances. From the results, it is assumed that peat humic acid has no polycyclic ring systems as the aromatic structure, and that the polycyclic aromatic hydrocarbons produced by zinc-dust distillation were formed by a rearrangement and condensation of oxygen containing structures during the reaction.

  3. Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue.

    Science.gov (United States)

    Barbaro, Elena; Zangrando, Roberta; Barbante, Carlo; Gambaro, Andrea

    2016-01-01

    Domoic acid (DA), a neurotoxic amino acid produced by diatoms, is the main cause of amnesic shellfish poisoning (ASP). In this work, we propose a very simple and fast analytical method to determine DA in mussel tissue. The method consists of two consecutive extractions and requires no purification steps, due to a reduction of the extraction of the interfering species and the application of very sensitive and selective HILIC-MS/MS method. The procedural method was validated through the estimation of trueness, extract yield, precision, detection, and quantification limits of analytical method. The sample preparation was also evaluated through qualitative and quantitative evaluations of the matrix effect. These evaluations were conducted both on the DA-free matrix spiked with known DA concentration and on the reference certified material (RCM). We developed a very selective LC-MS/MS method with a very low value of method detection limit (9 ng g(-1)) without cleanup steps. PMID:26904720

  4. An Amperometric Biosensor for Uric Acid Determination Prepared From Uricase Immobilized in Polyaniline-Polypyrrole Film

    Directory of Open Access Journals (Sweden)

    Fatma Arslan

    2008-09-01

    Full Text Available A new amperometric uric acid biosensor was developed by immobilizing uricase by a glutaraldehyde crosslinking procedure on polyaniline-polypyrrole (pani-ppy composite film on the surface of a platinum electrode. Determination of uric acid was performed by the oxidation of enzymatically generated H2O2 at 0.4 V vs. Ag/AgCl. The linear working range of the biosensor was 2.5×10-6 – 8.5×10-5 M and the response time was about 70 s. The effects of pH, temperature were investigated and optimum parameters were found to be 9.0, 55 oC, respectively. The stability and reproducibility of the enzyme electrode have been also studied.

  5. Using Capillary Electrophoresis to Determine the Purity of Acetylsalicylic Acid Synthesized in the Undergraduate Laboratory

    Science.gov (United States)

    Welder, Frank; Colyer, Christa L.

    2001-11-01

    Capillary electrophoresis (CE), although a powerful analytical tool, has found only limited application in undergraduate laboratory study. In an effort to expose freshman and sophomore chemistry students to this technique, thereby giving them practical instrumental experience early in their careers, we propose to use CE in the analysis of student-synthesized acetylsalicylic acid (ASA). The synthesis of ASA from salicylic acid (SA) is a routine undergraduate laboratory, although students rarely have the opportunity to test the purity of their product. The CE method described herein provides students with a method to test purity and yield of their product and to determine the effect of aging on their sample. CE can accomplish this in a short period of time, with minimal disruption to the regular laboratory curriculum. Optimized separation conditions, limits of detection, and linear range for ASA and SA are also given.

  6. Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

    Directory of Open Access Journals (Sweden)

    Elena Barbaro

    2016-01-01

    Full Text Available Domoic acid (DA, a neurotoxic amino acid produced by diatoms, is the main cause of amnesic shellfish poisoning (ASP. In this work, we propose a very simple and fast analytical method to determine DA in mussel tissue. The method consists of two consecutive extractions and requires no purification steps, due to a reduction of the extraction of the interfering species and the application of very sensitive and selective HILIC-MS/MS method. The procedural method was validated through the estimation of trueness, extract yield, precision, detection, and quantification limits of analytical method. The sample preparation was also evaluated through qualitative and quantitative evaluations of the matrix effect. These evaluations were conducted both on the DA-free matrix spiked with known DA concentration and on the reference certified material (RCM. We developed a very selective LC-MS/MS method with a very low value of method detection limit (9 ng g−1 without cleanup steps.

  7. Determination of the Thermal Decomposition Products of Terephthalic Acid by Using Curie-Point Pyrolyzer

    Science.gov (United States)

    Begüm Elmas Kimyonok, A.; Ulutürk, Mehmet

    2016-04-01

    The thermal decomposition behavior of terephthalic acid (TA) was investigated by thermogravimetry/differential thermal analysis (TG/DTA) and Curie-point pyrolysis. TG/DTA analysis showed that TA is sublimed at 276°C prior to decomposition. Pyrolysis studies were carried out at various temperatures ranging from 160 to 764°C. Decomposition products were analyzed and their structures were determined by gas chromatography-mass spectrometry (GC-MS). A total of 11 degradation products were identified at 764°C, whereas no peak was observed below 445°C. Benzene, benzoic acid, and 1,1‧-biphenyl were identified as the major decomposition products, and other degradation products such as toluene, benzophenone, diphenylmethane, styrene, benzaldehyde, phenol, 9H-fluorene, and 9-phenyl 9H-fluorene were also detected. A pyrolysis mechanism was proposed based on the findings.

  8. Multiwavelength spectrophotometric determination of acidity constants of 1-(2-thiazolylazo)-2-naphthol in methanol-water mixtures

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The acid-base properties of 1-(2-thiazolylazo)-2-naphthol (TAN) in mixtures of methanol-water at 25 ℃ and an ionic strength of 0.1 mol/L are studied by a multi-wavelength spectrophotometric method. The acidity constants of all related equilibria are estimated using the whole spectral fitting of the collected data to an established factor analysis model. DATAN program was used for determination of acidity constants. The corresponding pKa values in methanol-water mixtures were determined. There is a linear relationship between acidity constants and the mole fraction of methanol in the solvent mixtures.

  9. Determination and Correlation of Solubility for D-Xylose in Volatile Fatty Acid Solvents

    Institute of Scientific and Technical Information of China (English)

    李涛; 陈飞雄; 江振西; 任保增

    2014-01-01

    The solubility of D-xylose in formic acid and binary solvents of formic acid with formic acid and acetic acid, propionic acid, n-butyric acid or isobutyric acid was measured in the temperature range from 300.35 to 325.05 K using the synthetic method by a laser monitoring technique at atmospheric pressure. The solid-liquid equilibrium data will provide essential support for industrial design and further theoretical study. The experimental data show that the solubility of D-xylose in formic acid and in the mixtures of formic acid+acetic acid (1︰1), formic acid+propionic acid (1︰1), formic acid+n-butyric acid (1︰1), and formic acid+isobutyric acid (1︰1) increases with temperature. The Apelblat equation, theλh model, and the ideal solution equation correlate the solubility data well.

  10. Adsorption of tannic acid on polyelectrolyte monolayers determined in situ by streaming potential measurements.

    Science.gov (United States)

    Oćwieja, M; Adamczyk, Z; Morga, M

    2015-01-15

    Physicochemical characteristics of tannic acid (tannin) suspensions comprising its stability for a wide range of ionic strength and pH were thoroughly investigated using UV-vis spectrophotometry, dynamic light scattering and microelectrophoretic measurements. These studies allowed to determine the hydrodynamic diameter of the tannic acid that was 1.63 nm for the pH range 3.5-5.5. For pH above 6.0 the hydrodynamic diameter significantly decreased as a result of the tannin hydrolysis. The electrophoretic mobility measurements confirmed that tannic acid is negatively charged for these values of pH and ionic strength 10(-4)-10(-2) M. Therefore, in order to promote adsorption of tannin molecules on negatively charged mica, the poly(allylamine hydrochloride) (PAH) supporting monolayers were first adsorbed under diffusion transport conditions. The coverage of polyelectrolyte monolayers was regulated by changing bulk concentration of PAH and the adsorption time. The electrokinetic characteristics of bare and PAH-covered mica were determined using the streaming potential measurements. The zeta potential of these PAH monolayers was highly positive, equal to 46 mV for ionic strength of 10(-2) M. The kinetics of tannin adsorption on these PAH supporting monolayers was evaluated by the in situ the streaming potential measurements. The zeta potential of PAH monolayers abruptly decreases with the adsorption of tannin molecules that was quantitatively interpreted in terms of the three-dimensional electrokinetic model. The acid-base characteristics of tannin monolayers were acquired via the streaming potential measurements for a broad range of pH. The obtained results indicate that it is possible to control adsorption of tannin on positively charged surfaces in order to designed new multilayer structures of desirable electrokinetic properties and stability.

  11. Derivatization/chromophore introduction of tranexamic acid and its HPLC determination in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    M. Ashfaq

    2015-04-01

    Full Text Available A viable cost-effective and isocratic approach employing C-18 column (250 mm × 4.6 mm, 5 μm based HPLC has been utilized to separate and estimate the drug, tranexamic acid in pharmaceutical formulations. Tranexamic acid contains no π-electrons to act as fluorophore or chromophore hence pre-column derivatization was performed with benzene sulfonyl chloride in aqueous medium at room temperature. The derivatized drug was then estimated using C-18 column by exploiting a 25:75 (v/v solvent mixture of acetonitrile and 0.1 M ammonium acetate (pH 5.0 as the mobile phase. The flow rate of mobile phase was 1 mL/min and detection was performed at a wavelength of 232 nm using UV detector. Retention time of tranexamic acid was 4.42 min. The method followed linear regression equation in the concentration range of 1–100 μg/mL with co-efficient of determination equal to 0.9994. The limit of detection and limit of quantitation were 0.3 and 1 μg/mL, respectively. The relative standard deviation and recovery ranges for tranexamic acid were found to be 0.11–2.47% and 97.60–103.25%, respectively. The suggested method is very sensitive and may have the potential to be used for tranexamic acid detection in medicinal formulations.

  12. A Doped Polyaniline Modified Electrode Amperometric Biosensor for Gluconic Acid Determination in Grapes

    Directory of Open Access Journals (Sweden)

    Donatella Albanese

    2014-06-01

    Full Text Available In winemaking gluconic acid is an important marker for quantitative evaluation of grape infection by Botrytis cinerea. A screen-printed amperometric bienzymatic sensor for the determination of gluconic acid based on gluconate kinase (GK and 6-phospho-D-gluconate dehydrogenase (6PGDH coimmobilized onto polyaniline/poly (2-acrylamido-2-methyl-1-propanesulfonic acid; PANI-PAAMPSA is reported in this study. The conductive polymer electrodeposed on the working electrode surface allowed the detection of NADH at low potential (0.1 V with a linear range from 4 × 10−3 to 1 mM (R2 = 0.99 and a sensitivity of 419.44 nA∙mM−1. The bienzymatic sensor has been optimized with regard to GK/6PGDH enzymatic unit ratio and ATP/NADP+ molar ratio which resulted equal to 0.33 and 1.2, respectively. Under these conditions a sensitivity of 255.2 nA∙mM−1, a limit of detection of 5 μM and a Relative Standard Deviation (RSD of 4.2% (n = 5 have been observed. Finally, the biosensor has been applied for gluconic acid measurements in must grape samples and the matrix effect has been taken into consideration. The results have been compared with those obtained on the same samples with a commercial kit based on a spectrophotometric enzyme assay and were in good agreement, showing the capability of the bienzymatic PANI-PAAMPSA biosensor for gluconic acid measurements and thus for the evaluation of Botrytis cinerea infection in grapes.

  13. [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.

  14. New method for the direct determination of dissolved Fe(III) concentration in acid mine waters

    Science.gov (United States)

    To, T.B.; Nordstrom, D.K.; Cunningham, K.M.; Ball, J.W.; McCleskey, R.B.

    1999-01-01

    A new method for direct determination of dissolved Fe(III) in acid mine water has been developed. In most present methods, Fe(III) is determined by computing the difference between total dissolved Fe and dissolved Fe(II). For acid mine waters, frequently Fe(II) >> Fe(III); thus, accuracy and precision are considerably improved by determining Fe(III) concentration directly. The new method utilizes two selective ligands to stabilize Fe(III) and Fe(II), thereby preventing changes in Fe reduction-oxidation distribution. Complexed Fe(II) is cleanly removed using a silica-based, reversed-phase adsorbent, yielding excellent isolation of the Fe(III) complex. Iron(III) concentration is measured colorimetrically or by graphite furnace atomic absorption spectrometry (GFAAS). The method requires inexpensive commercial reagents and simple procedures that can be used in the field. Calcium(II), Ni(II), Pb(II), AI(III), Zn(II), and Cd(II) cause insignificant colorimetric interferences for most acid mine waters. Waters containing >20 mg of Cu/L could cause a colorimetric interference and should be measured by GFAAS. Cobalt(II) and Cr(III) interfere if their molar ratios to Fe(III) exceed 24 and 5, respectively. Iron(II) interferes when its concentration exceeds the capacity of the complexing ligand (14 mg/L). Because of the GFAAS elemental specificity, only Fe(II) is a potential interferent in the GFAAS technique. The method detection limit is 2 ??g/L (40 nM) using GFAAS and 20 ??g/L (0.4 ??M) by colorimetry.A new method for direct determination of dissolved Fe(III) in acid mine water has been developed. In most present methods, Fe(III) is determined by computing the difference between total dissolved Fe and dissolved Fe(II). For acid mine waters, frequently Fe(II)???Fe(III); thus, accuracy and precision are considerably improved by determining Fe(III) concentration directly. The new method utilizes two selective ligands to stabilize Fe(III) and Fe(II), thereby preventing changes

  15. Determination of Organic Acids in Root Exudates by High Performance Liquid Chromatography:Ⅲ.Effects of Interfering Factors

    Institute of Scientific and Technical Information of China (English)

    SHENJIANBO; ZHANGFUSUO; 等

    1999-01-01

    A solution culture experiment was conducted to investigate the effects of collection time and interfering ions on separation and determination of low-molecular-weight organic acids in root exudates of soybean using the method for directly collecting root exudates.The suitable cooection time of root exudates and the interferiung ions affecting organic acid determination were determined.The method for removing the interfering ions was established and analyzed.The release amount of root exudates increased with the increase of collection time from 0 to 120min but decreased with increasing of collection time from 120to 240min.The maximum exuding amounts of organic acids were observed in root exudates at the collection time of 120min.There was a significant difference of organic acid components between the treatments of collection time of 120min and 240min,Citric acid was founnd only in the treatment of 120min collection time,NO3- was the main interfering ion in organic acid determination and had the same retention time as oxalic acid.Anion exchange resin(SAX)properly treated by HPLC(high performance liquid chromatography)solvent could remove NO3- anion in sample solution of root exudates,thus enhancing the recoveries of organic acids in root exudates.There was no significant effect of the chemicals added into sample solution such as H3PO4,SAX and KNO3 on the retention time of organic acids.

  16. New method for the direct determination of dissolved Fe(III) concentration in acid mine waters

    International Nuclear Information System (INIS)

    A new method for direct determination of dissolved Fe(III) in acid mine water has been developed. In most present methods, Fe(III) is determined by computing the difference between total dissolved Fe and dissolved Fe(II). For acid mine waters, frequently Fe(II) much-gt Fe(III); thus, accuracy and precision are considerably improved by determining Fe(III) concentration directly. The new method utilizes two selective ligands to stabilize Fe(III) and Fe(II), thereby preventing changes in Fe reduction-oxidation distribution. Complexed Fe(II) is cleanly removed using a silica-based, reversed-phase adsorbent, yielding excellent isolation of the Fe(III) complex. Iron(III) concentration is measured colorimetrically or by graphite furnace atomic absorption spectrometry (GFAAS). The method requires inexpensive commercial reagents and simple procedures that can be used in the field. Calcium(II), Ni(II), Pb(II), Al(III), Zn(II), and Cd(II) cause insignificant colorimetric interferences for most acid mine waters. Waters containing >20 mg of Cu/L could cause a colorimetric interference and should be measured by GFAAS. Cobalt(II) and Cr(III) interfere if their molar ratios to Fe(III) exceed 24 and 5, respectively. Iron(II) interferes when its concentration exceeds the capacity of the complexing ligand. Because of the GFAAS elemental specificity, only Fe(II) is a potential interferent in the GFAAS technique. The method detection limit is 2 microg/L using GFAAS and 20 microg/L by colorimetry

  17. Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

    Science.gov (United States)

    Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

    2014-12-01

    Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane.

  18. Effect of intraarticular osmic acid on synovial membrane volume and inflammation, determined by magnetic resonance imaging

    DEFF Research Database (Denmark)

    Østergaard, Mikkel; Stoltenberg, M; Gideon, P;

    1995-01-01

    The changes in MR-determined synovial membrane volume, early synovial enhancement, and cartilage and bone erosions after osmic acid knee synovectomy were studied. Gadolinium-DTPA enhanced magnetic resonance imaging (MRI) of 18 knees with persistent arthritis was performed before and 1 month after...... treatment. The synovial membrane volume was significantly reduced (median -52%) in all 9 patients brought into clinical remission (p < 0.01), while no significant change was found in patients with clinical relapse. The early synovial enhancement was not significantly changed. MRI revealed progressive...

  19. New Method for the Determination of Ionization Constants of Polyprotic Weak Acid

    Institute of Scientific and Technical Information of China (English)

    王静康; 郝红勋

    2003-01-01

    A new method for the determination of ionization constants of polyprotic weak acids is presented.Based on dissociation equilibrium, mass balance and charge balance, the mathematic model is established and the non-linear least-squares Gauss-Newton method is applied to numerically solve the model equations. In order to get the concentration of hydrogen ion, the Debye-Huckel equation is used to calculate its activity coefficient. The ionization constants of H2SO3 and H2C2O4 obtained by this method are in good agreement with the literature values.

  20. Determination of the amino acid requirements for a protein hinge in triosephosphate isomerase.

    OpenAIRE

    Sun, J.; Sampson, N. S.

    1998-01-01

    We have determined the sequence requirements for a protein hinge in triosephosphate isomerase. The codons encoding the hinge at the C-terminus of the active-site lid of triosephosphate isomerase were replaced with a genetic library of all possible 8,000 amino acid combinations. The most active of these 8,000 mutants were selected using in vivo complementation of a triosephosphate isomerase deficient strain of E. coli, DF502. Approximately 3% of the mutants complement DF502 with an activity th...

  1. A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

    Science.gov (United States)

    Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

    2013-03-01

    Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. PMID:23381802

  2. Simultaneous determination of niacin, niacinamide and nicotinuric acid in human plasma.

    Science.gov (United States)

    Pfuhl, P; Kärcher, U; Häring, N; Baumeister, A; Tawab, Mona Abdel; Schubert-Zsilavecz, M

    2005-01-01

    A sensitive, specific, accurate, and reproducible HPLC/MS-method for the simultaneous quantitative determination of niacin (NA) and its main metabolites niacinamide (NAM) and nicotinuric acid (NUR) in human plasma using chinolin-3-carboxylic acid as an internal standard was developed and validated according to international guidelines for method validation. All analytes and the internal standard were separated from acidified plasma by solid phase extraction. Afterwards the extracted samples were analyzed by HPLC/MS in the positive electrospray ionization mode (ESI) and selected ion monitoring (SIM). The total run time was 7 min between injections. The assay had a lower limit of quantification of 50.0 ng/mL for each analyte using 1 mL of plasma. The calibration curves were linear in the measured range between 50.0 and 750 ng/mL plasma. The overall precision and accuracy for all concentrations of quality controls and standards was better than 15%. No indications were found for possible instabilities of niacin, niacinamide and nicotinuric acid in plasma at -20 degrees C, in the extraction solvent or after repeated thawing/freezing cycles. In stabilities were observed in whole blood and in plasma at room temperature. The recovery of the extraction method ranged from 86 to 89% for the three analytes.

  3. Simultaneous determination of prenylflavonoid and hop bitter acid in beer lee by HPLC-DAD-MS.

    Science.gov (United States)

    Kao, T H; Wu, G Y

    2013-11-15

    An HPLC-DAD-MS method with high accuracy and precision was developed for determination of prenylflavonoids and hop bitter acids in beer lee, a by-product from beer brewing process. Four prenylflavonoids and nine hop bitter acids can be simultaneously separated in 29 min using a Thermo HyPURITY C18 column in combination with diode array dectector and mass spectrometer with HPLC solvent gradient system of phosphoric acid aqueous solution at pH 1.6 and acetonitrile at a flow rate of 1.5 mL/min and detection wavelength at 314 nm. Beer lee is found to contain isoxanthohumol (36.2 μg/g), xanthohumol (29.6 μg/g), 8-prenylnaringenin (7.84 μg/g), 6-prenylnaringenin (19.2 μg/g), cohumulone (44.7 μg/g), humulone (123 μg/g), adhumulone (21.8 μg/g), colupulone (44.2 μg/g), lupulone (33.2 μg/g), and adlupulone (5.76 μg/g).

  4. Determination of acetylsalicylic acid in commercial tablets by SERS using silver nanoparticle-coated filter paper

    Science.gov (United States)

    Sallum, Loriz Francisco; Soares, Frederico Luis Felipe; Ardila, Jorge Armando; Carneiro, Renato Lajarim

    2014-12-01

    In this work, filter paper was used as a low cost substrate for silver nanoparticles in order to perform the detection and quantification of acetylsalicylic acid by SERS in a commercial tablet. The reaction conditions were 150 mM of ammonium hydroxide, 50 mM of silver nitrate, 500 mM of glucose, 12 min of the reaction time, 45 °C temperature, pretreatment with ammonium hydroxide and quantitative filter paper (1-2 μm). The average size of silver nanoparticles deposited on the paper substrate was 180 nm. Adsorption time of acetylsalicylic acid on the surface of the silver-coated filter paper was studied and an adsorption time of 80 min was used to build the analytical curve. It was possible to obtain a calibration curve with good precision with a coefficient of determination of 0.933. The method proposed in this work was capable to quantify acetylsalicylic acid in commercial tablets, at low concentration levels, with relative error of 2.06% compared to the HPLC. The preparation of filter paper coated with silver nanoparticles using Tollen's reagent presents several advantages such as low cost of synthesis, support and reagents; minimum amount of residuals, which are easily treated, despite the SERS spectroscopy presenting fast analysis, with low sample preparation and low amount of reactants as in HPLC analysis.

  5. Estudio numerico y experimental del proceso de soldeo MIG sobre la aleacion 6063--T5 utilizando el metodo de Taguchi

    Science.gov (United States)

    Meseguer Valdenebro, Jose Luis

    improvement on mechanical properties in aluminum metal joint. Los procesos de soldadura por arco electrico representan unas de las tecnicas mas utilizadas en los procesos de fabricacion de componentes mecanicos en la industria moderna. Los procesos de soldeo por arco se han adaptado a las necesidades actuales, haciendose un modo de fabricacion flexible y versatil. Los resultados obtenidos numericamente en el proceso de soldadura son validados experimentalmente. Los principales metodos numericos mas empleados en la actualidad son tres, metodo por diferencias finitas, metodos por elementos finitos y metodo por volumenes finitos. El metodo numerico mas empleado para el modelado de uniones soldadas, es el metodo por elementos finitos, debido a que presenta una buena adaptacion a las condiciones geometricas y de contorno ademas de que existe una diversidad de programas comerciales que utilizan el metodo por elementos finitos como base de calculo. Este trabajo de investigacion presenta un estudio experimental de una union soldada mediante el proceso MIG de la aleacion de aluminio 6063-T5. El metodo numerico se valida experimentalmente aplicando el metodo de los elementos finitos con el programa de calculo ANSYS. Los resultados experimentales obtenidos son: las curvas de enfriamiento, el tiempo critico de enfriamiento t4/3, geometria del cordon, microdurezas obtenidas en la union soldada, zona afectada termicamente y metal base, dilucion del proceso, areas criticas intersecadas entre las curvas de enfriamiento y la curva TTP. Los resultados numericos son: las curvas del ciclo termico, que representan tanto el calentamiento hasta alcanzar la temperatura maxima y un posterior enfriamiento. Se calculan el tiempo critico de enfriamiento t4/3, el rendimiento termico y se representa la geometria del cordon obtenida experimentalmente. La zona afectada termicamente se obtiene diferenciando las zonas que se encuentran a diferentes temperaturas, las areas criticas intersecadas entre las

  6. Atlas de aves: Un metodo para documentar distribucion y seguir poblaciones

    Science.gov (United States)

    Robbins, C.S.; Dowell, B.A.; Dawson, D.K.; Alvarez-Lopez, Humberto; Kattan, Gustavo; Murcia, Carolina

    1988-01-01

    Los Atlas de Aves son proyectos nacionales o regionalies para trazar en mapas la distribucion en reproduccion de cada especie de ave. Ese procedimiento se esta usando en Europa, Australia, Nueva Zelanda, Norteamerica, y partes de Africa. El tama?o de los cuadrados varia de medio grado de latitud y Iongitud hasta 5 x 5 km. El trabajo de campo de cada proyecto exige aproxlmadamente cinco a?os, pero los aficionados pueden llevar a cabo la mayor parte del trabajo. Es posible almacenar los resultados en un computador personal. Hay muchos beneficios: (I) se presenta la distribucion corriente de las aves de la nacion, del estado, o de la Iocalidad; (2) se desarrolla nueva informacion especialmente sobre especies raras o en peligro; (3) se descubren areas que tienen una avlfauna sobresaliente o habitats raros y ayuda a su proteccion, (4) se documentan cambios de dlstribucion; (5) se pueden usar para documentar cambios de poblacion, especialmente en los tropicos donde otros metodos son mas dificiles de usar porque hay muchas especies y no hay muchos observadores calificados en la identificacion de sonidos de las aves; (6) son proyectos buenos de investigacion para estudiantes graduados; (7) los turistas y los jefes de excursiones de historia natural pueden contribuir con muchas informaciones

  7. A modified approach for rapid determination of the quality of industrially produced P-33 orthophosphoric acid preparations

    International Nuclear Information System (INIS)

    In this work we have developed an approach to rapidly estimate the quality of P-33 labeled Orthophosphoric Acid (carrier free) in industrial production. The method was created to determine the values of specific radioactivity for both Orthophosphoric acid and gamma-Adenosine 5'-Triphosphate (ATP) by means of enzymatic ATP synthesis in equal molar ratio conditions for two main substrates (radioactive Orthophosphoric acid and ADP) with following chromatography of the reaction mixture on the PEI-cellulose micro column

  8. Rapid Determination of HAAs Formation Potential of the Reaction of Humic Acid with Chlorine or Chlorine Dioxide

    Institute of Scientific and Technical Information of China (English)

    ZHU Zhi-liang; GE Yuan-xin; ZHANG Rong-hua; MA Hong-mei; HAO Jian-fu

    2007-01-01

    On the basis of gas chromatography(GC) coupled with a short capillary column and an electron capture detector(ECD), a simple and rapid method for the determination of five haloacetic acids(HAAs) in drinking water was developed by the optimization of derivation conditions and the modification of gas chromatographic program. HAAs formation potential(HAAFP) of the reaction of humic acid with chlorine was determined via this method. The major advantages of the method are the simplicity of chromatographic temperature program and the short run time of GC. Dichloroacetic acid(DCAA) and Trichloroacetic acid(TCAA), which were detected in the determination of HAAFP, were rapidly formed in the first 72 h of the reaction of humic acid with chlorine. HAAFP of the reaction of humic acid with chlorine increased with the increase in the concentrations of humic acid and chlorine. The average HAAFP of the reaction of humic acid with chlorine was 39.9 μg/mg TOC under the experimental conditions. When the concentration of humic acid was 4 mg/L, the concentration of HAAs, which were produced in the reaction of humic acid with chorine, may exceed MCL of 60 μg/L HAAs as the water quality standards for urban water supply of China and the first stage of US EPA disinfection/disinfection by-products(D/DBP) rule; when the concentration of humic acid was 2 mg/L, the concentration of HAAs may exceed MCL of 30 μg/L HAAs for the second stage of US EPA D/DBP rule. When humic acid was reacted with chlorine dioxide, only DCAA was detected with a maximum concentration of 3.3 μg/L at a humic acid content of 6 mg/L. It was demonstrated that the substitution of chlorine dioxide for chorine may entirely or partly control the formation of HAAs and effectively reduce the health risk associated with disinfected drinking water.

  9. Determination of fruit characteristics, fatty acid profile and total antioxidant capacity ofMespilus germanica L. fruit

    Institute of Scientific and Technical Information of China (English)

    Hale Seilmi Canbay; Ersin Atay; Serdal Ot

    2015-01-01

    Objective:To determine fruit characteristics, fatty acid profile and total antioxidant capacitiy of first culturedMespilus germanica L. Methods: A total of15 fruits were taken randomly from four directions of adult trees.Then the physical and chemical properties of first cultured medlar fruit (Istanbul/Turkey) were measured by using refractometer, colorimeter, spectrophotometer and gas chromatograph mass spectrometer, respectivly. Results: In the fruit studied, the results showed that palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid, arachidic acid and behenic acid were the most abundant fatty acids (FAs), and the main FA was palmitic acid [(35.35 ± 1.20)%]. The percentage of linoleic acid and stearic acid in this fruit oil were (29.10 ± 1.70)% and(8.53 ± 0.25)%, respectively. As a result of the analysis, the total antioxidant capacity of medlar fruit was (1.1 ± 0.2) mmol trolox equivalents/L. Conclusions: The present study has demonstrated the concentrations of FAs and the antioxidantive capacity of first cultured Istanbul medlar fruits by using many tested methods. It is proved that in our daily life, medlar fruit plays a significant role with its nutrition and health effect.

  10. [Rapid determination of fatty acids in soybean oils by transmission reflection-near infrared spectroscopy].

    Science.gov (United States)

    Song, Tao; Zhang, Feng-ping; Liu, Yao-min; Wu, Zong-wen; Suo, You-rui

    2012-08-01

    In the present research, a novel method was established for determination of five fatty acids in soybean oil by transmission reflection-near infrared spectroscopy. The optimum conditions of mathematics model of five components (C16:0, C18:0, C18:1, C18:2 and C18:3) were studied, including the sample set selection, chemical value analysis, the detection methods and condition. Chemical value was analyzed by gas chromatography. One hundred fifty eight samples were selected, 138 for modeling set, 10 for testing set and 10 for unknown sample set. All samples were placed in sample pools and scanned by transmission reflection-near infrared spectrum after sonicleaning for 10 minute. The 1100-2500 nm spectral region was analyzed. The acquisition interval was 2 nm. Modified partial least square method was chosen for calibration mode creating. Result demonstrated that the 1-VR of five fatty acids between the reference value of the modeling sample set and the near infrared spectrum predictive value were 0.8839, 0.5830, 0.9001, 0.9776 and 0.9596, respectively. And the SECV of five fatty acids between the reference value of the modeling sample set and the near infrared spectrum predictive value were 0.42, 0.29, 0.83, 0.46 and 0.21, respectively. The standard error of the calibration (SECV) of five fatty acids between the reference value of testing sample set and the near infrared spectrum predictive value were 0.891, 0.790, 0.900, 0.976 and 0.942, respectively. It was proved that the near infrared spectrum predictive value was linear with chemical value and the mathematical model established for fatty acids of soybean oil was feasible. For validation, 10 unknown samples were selected for analysis by near infrared spectrum. The result demonstrated that the relative standard deviation between predict value and chemical value was less than 5.50%. That was to say that transmission reflection-near infrared spectroscopy had a good veracity in analysis of fatty acids of soybean oil.

  11. Determination of soluble solid content and acidity of loquats based on FT-NIR spectroscopy

    Institute of Scientific and Technical Information of China (English)

    Xia-ping FU; Jian-ping LI; Ying ZHOU; Yi-bin YING; Li-juan XIE; Xiao-ying NIU; Zhan-ke YAN; Hai-yan YU

    2009-01-01

    The near infrared (NIR) spectroscopy technique has been applied in many fields because of its advantages of simple preparation,fast response,and non-destructiveness.We investigated the potential of NIR spectroscopy in diffuse reflectance mode for determining the soluble solid content (SSC) and acidity (pH) of intact loquats.Two cultivars of loquats (Dahongpao and Jiajiaozhong) harvested from two orchards (Tangxi and Chun'an,Zhejiang,China) were used for the measurement of NIR spectra between 800 and 2500 nm.A total of 400 loquats (100 samples of each cultivar from each orchard) were used in this study.Relationships between NIR spectra and SSC and acidity of ioquats were evaluated using partial least square (PLS) method.Spectra preprocessing options included the first and second derivatives,multiple scatter correction (MSC),and the standard normal variate (SNV).Three separate spectral windows identified as full NIR (800-2500 nm),short NIR (800~1100 nm),and long NIR (1100~2500 nm) were studied in factorial combination with the preprocessing options.The models gave relatively good predictions of the SSC of loquats,with root mean square error of prediction (RMSEP) values of 1.21,1.00,0.965,and 1.16 °Brix for Tangxi-Dahongpao,Tangxi-Jiajiaozhong,Chun'an-Dahongpao,and Chun'an-Jiajiaozhong,respectively.The acidity prediction was not satisfactory,with the RMSEP of 0.382,0.194,0.388,and 0.361 for the above four loquats,respectively.The results indicate that NIR diffuse reflectance spectroscopy can be used to predict the SSC and acidity of loquat fruit.

  12. Solid phase extraction and spectrophotometric determination of palladium with 2-(2-quinolylazo-5-diethylaminobenzoic acid

    Directory of Open Access Journals (Sweden)

    WEIZU YANG

    2006-07-01

    Full Text Available Asensitive, selective and rapid method for the determination of palladium based on the rapid reaction of palladium(II with 2-(2-quinolylazo-5-diethylaminobenzoic acid (QADEAB and the solid phase extraction of the Pd(II –QADEAB chelate with a reversed phase polymer-based C18 cartridge was developed. In the presence of 0.05 – 0. 5 mol/L of hydrochloric acid solution and cetyl trimethylammonium bromide (CTAB medium, QADEAB reacts with palladium(II to form a violet complex with a mole ratio 1:2 (palladium to QADEAB. The chelate was enriched by solid phase extraction with a reversed phase polymer-based C18 cartridge. An enrichment factor of 200 was obtained by elution of the chelate form the cartridge with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate in the isopentyl alcohol medium was 1.43 × 105 L mol-1 cm-1 at 628 nm. Beer’s law was obeyed in the range of 0.01 – 1.2 mg/mL. The relative standard deviation for eleven replicate samples at the 0.2 mg/L level was 2.18 %. The attained detection limit amounted to 0.02 mg/L in the original samples. This method was applied to the determination of palladium in environmental samples with good results.

  13. A Modified Fluorimetric Method for Determination of Hydrogen Peroxide Using Homovanillic Acid Oxidation Principle

    Directory of Open Access Journals (Sweden)

    Biswaranjan Paital

    2014-01-01

    Full Text Available Hydrogen peroxide (H2O2 level in biological samples is used as an important index in various studies. Quantification of H2O2 level in tissue fractions in presence of H2O2 metabolizing enzymes may always provide an incorrect result. A modification is proposed for the spectrofluorimetric determination of H2O2 in homovanillic acid (HVA oxidation method. The modification was included to precipitate biological samples with cold trichloroacetic acid (TCA, 5% w/v followed by its neutralization with K2HPO4 before the fluorimetric estimation of H2O2 is performed. TCA was used to precipitate the protein portions contained in the tissue fractions. After employing the above modification, it was observed that H2O2 content in tissue samples was ≥2 fold higher than the content observed in unmodified method. Minimum 2 h incubation of samples in reaction mixture was required for completion of the reaction. The stability of the HVA dimer as reaction product was found to be >12 h. The method was validated by using known concentrations of H2O2 and catalase enzyme that quenches H2O2 as substrate. This method can be used efficiently to determine more accurate tissue H2O2 level without using internal standard and multiple samples can be processed at a time with additional low cost reagents such as TCA and K2HPO4.

  14. [Determination of ellagic acid, flavonoids and goshonoside-F5 in Rubi Fructus by HPLC].

    Science.gov (United States)

    He, Jian-Ming; Sun, Nan; Wu, Wen-Dan; Fan, Li-Jiao; Guo, Mei-Li

    2013-12-01

    High-performance liquid chromatographic coupled with variable wavelength detection (HPLC-VWD) has been developed for simultaneous determination of 5 analytes including ellagic acid, quercetin, kaempferol-3-O-beta-D-rutinoside, tiliroside and kaempferol, and high-performance liquid chromatographic with an evaporative light scattering detector (HPLC-ELSD) has been established to determine goshonoside-F5 in extract of Rubi Fructus. Chromatographic separations were carried out on an Agilent ZORBAX SB-C18 column (4.6 mm x 250 mm, 5.0 microm). All calibration curves of reference standards revealed good linearity (R2 > 0.999 5) within the concentration ranges tested. The method limits of detection ranged 0.297-90.144 ng and the method limits ofquantitation ranged 0.990-300.480 ng, respectively. Recoveries of 6 analytes were from 97.11% to 101.7%, with RSD less than 2.1%. The result shows that amounts of the 6 analytes in the samples from 16 localities were found to be different. The higher latitude of growing environment, the more ellagic acid in herb. The content of total flavonoids in sample from east localities were higher than that in middle and west localities, and the content of goshonoside-F5 in Bozhou, Anhui province was higher than others. This method was found to be simple, accurate, sensitive with good repeatability. Those results might serve as a sound foundation for further study, quality control and application of Rubi Fructus.

  15. Determination of acrolein, ethanol, volatile acidity, and copper in different samples of sugarcane spirits

    Directory of Open Access Journals (Sweden)

    José Masson

    2012-09-01

    Full Text Available Seventy-one samples of sugarcane spirits from small and average size stills produced in the northern and southern Minas Gerais (Brazil were analyzed for acrolein using HPLC (High Performance Liquid Chromatography. Ethanol and copper concentrations and volatile acidity were also determined according to methods established by the Ministry of Agriculture, Livestock and Supply (MAPA. A total of 9.85% of the samples tested showed levels of acrolein above the legal limits, while the copper concentrations of 21.00% of the samples and the volatile acidity of 8.85% of the samples were higher than the limits established by the Brazilian legislation. The concentration of acrolein varied from 0 to 21.97 mg.100 mL-1 of ethanol. However, no significant difference at 5% of significance was observed between the samples produced in the northern and southern Minas Gerais. The method used for determination of acrolein in sugarcane spirits involved the formation of a derivative with 2,4-dinitrophenylhydrazine (2,4-DNPH and subsequent analysis by HPLC.

  16. Determination of lactic acid with special emphasis on biosensing methods: A review.

    Science.gov (United States)

    Pundir, Chandra S; Narwal, Vinay; Batra, Bhawna

    2016-12-15

    Lactic acid (2-Hydroxypropanoic acid) is generated from pyruvic acid under anaerobic condition in skeletal muscles, brain, red blood cells, and kidney. Lactate in normal human subjects get cleared very quickly at a rate of 320mmol/L/hr, mostly by liver metabolism and re-conversion of lactate back to pyruvate. Measurement of lactate level in serum is required for the differential diagnosis and medical management of hyperlactatemia, cardiac arrest and resuscitation, sepsis, reduced renal excretion, hypoxia induced cancer, decreased extra hepatic metabolism, intestinal infarction and lactic acidosis. Determination of lactate is also important in dairy products and beverages to access their quality. Among the various methods available for detection of lactate, most are complicated, nonspecific, less sensitive and require time-consuming sample pretreatment, expensive instrumental set-up and trained persons to operate, specifically for chromatographic methods. Biosensing methods overcome these drawbacks, as these are simple, fast, specific and highly sensitive. Lactate biosensors reported so far, work optimally within 3-180s, between pH, 5.5-8.5 and temperature 22°C to 37°C and lactate concentration ranging from 10 to 2000µM. These biosensors have been employed to measure lactate level in embryonic cell culture, beverages, urine, and serum samples and reused upto 200-times within a period of 7-216 days. This review presents the principles, merits and demerits of various analytical methods for lactate determination with special emphasis on lactate biosensors. The future perspective for improvement of analytic performance of lactate biosensors are discussed. PMID:27476060

  17. Determination of Amino Acids in Single Human Lymphocytes after On-capillary Derivatization by Capillary Zone Electrophoresis with Electrochemical Detection

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Amino acids in individual human lymphocytes were determined by capillary zone electrophoresis with electrochemical detection after on-capillary derivatization. In order to inject cells easily, a cell injector was designed. Four amino acids (serine, alanine, taurine, and glycine) in single human lymphocytes have been identified. Quantitation has been accomplished through the use of calibration curves.

  18. Is the fatty acid composition of Daphnia galeata determined by the fatty acid composition of the ingested diet?

    NARCIS (Netherlands)

    Weers, P.M.M.; Siewertsen, K.; Gulati, R.D.

    1997-01-01

    1. The fatty acid (FA) composition of Daphnia galeata and their algal food was analysed and showed many similarities, however, some significant differences were also found in the relative abundance of the FA C16:4 omega 3 and docosahexaenoic acid (DHA). Their relative abundances were much lower in d

  19. Determination of fatty acids percentages and profile extracted from cuttlefish of Iranian coasts of Persian Gulf and Oman Sea

    Institute of Scientific and Technical Information of China (English)

    Yosief Ali Asadpour

    2014-01-01

    Objective: To determine the fatty acid profile extracted from cuttlefish of Persian Gulf and Oman Sea, including Ancistrocheirus, Enoploteuthidae, Cranchiidae, Ommastrephidae and Loliginidae. Methods:Oil was extracted by the Bligh and Dyer method. The fatty acid profile of the oil was determined by gas chromatography. Results:The results showed that (13±5)% of wet weight of cuttlefish is oil. The results also showed that cuttlefish oil has 29.40% saturated fatty acids and 23.70% single-band unsaturated fatty acids, and the total value of the unsaturated multiple-band is 40.20%, the contents of arachidonic acid 2.78%, linolenic acid 3.10%, linoleic acid 5.20%, docosahexaenoic acid 15.40%, and eicosapentaenoic acid 9.60% out of the total fatty acids of the same may be mentioned. Conclusions:The results of the current study described that cuttlefish is considered for the first time as the new and rich source of omega-3 and omega-6.

  20. Determination of Medronic Acid and Its Related Substances by Reversed-Phase High-Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    An isocratic liquid chromatographic method with evaporative light scattering detection (ELSD) was developed for the determination of medronic acid and its related substance. Volatile pentylamine was used as ion-pairing agent. Separations were performend

  1. Using the Chiral Organophosphorus Derivatizing Agents for Determination of the Enantiomeric Composition of Chiral Carboxylic Acids by 31PNMR Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    Chao CHE; Zhong Ning ZHANG; Gui Lan HUANG; Xin Xing WANG; Zhao Hai QIN

    2004-01-01

    The use of chiral organophosphorus derivatizing agents prepared in situ from chiral tartrate or chiral diamine for the 31PNMR determination of the enantiomeric composition of chiral carboxylic acids is described. The method is accurate, reliable and convenient.

  2. Simultaneous diffuse reflectance infrared determination of clavulanic acid and amoxicillin using multivariate calibration techniques.

    Science.gov (United States)

    Müller, Aline Lima Hermes; Picoloto, Rochele Sogari; Ferrão, Marco Flores; da Silva, Fabiana Ernestina Barcellos; Müller, Edson Irineu; Flores, Erico Marlon de Moraes

    2012-06-01

    A method for simultaneous determination of clavulanic acid (CA) and amoxicillin (AMO) in commercial tablets was developed using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and multivariate calibration. Twenty-five samples (10 commercial and 15 synthetic) were used as a calibration set and 15 samples (10 commercial and 5 synthetic) were used for a prediction set. Calibration models were developed using partial least squares (PLS), interval PLS (iPLS), and synergy interval PLS (siPLS) algorithms. The best algorithm for CA determination was siPLS model with spectra divided in 30 intervals and combinations of 2 intervals. This model showed a root mean square error of prediction (RMSEP) of 5.1 mg g(-1). For AMO determination, the best siPLS model was obtained with spectra divided in 10 intervals and combinations of 4 intervals. This model showed a RMSEP of 22.3 mg g(-1). The proposed method was considered as a suitable for the simultaneous determination of CA and AMO in commercial pharmaceuticals products.

  3. Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine.

    Science.gov (United States)

    Zhang, Xin; Wei, Youli; Ding, Yaping

    2014-07-01

    A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10(-8) to 1.2 × 10(-4) M with a detection limit (S/N=3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media. PMID:24952626

  4. Rapid fluorometric determination of perfluorooctanoic acid by its quenching effect on the fluorescence of quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Qi; Huang, Aizhen; Wang, Nan, E-mail: nwang@hust.edu.cn; Zheng, Guan; Zhu, Lihua

    2015-05-15

    Analysis of perfluorooctanoic acid (PFOA) usually requires a combination of high-performance liquid chromatography and mass spectrometry, which is expensive and time-consuming. In the present work, water-soluble CdS quantum dots (QDs) were employed to develop a simple and rapid fluorometric method for the determination of PFOA. Strongly fluorescent CdS QDs were prepared by using 3-mercaptopropionic acid (MPA) as a stabilizer. It was observed that PFOA strongly quenched the fluorescence emission of the MPA-CdS QDs because PFOA promotes the aggregation of MPA-CdS QDs through a fluorine–fluorine affinity interaction. Under optimum conditions, the fluorescence intensity of MPA-CdS QDs was observed to decrease linearly with an increase in the concentration of PFOA from 0.5 to 40 μmol L{sup −1}, with a limit of detection of 0.3 μmol L{sup −1}. This new method was successfully implemented for the analysis of PFOA-spiked textile samples, with recoveries ranging from 95% to 113%. - Highlights: • PFOA significantly quenched the fluorescence emission of quantum dots (QDs). • A rapid and simple fluorescence sensor was proposed for determining PFOA by QDs. • PFOA determination could be completed within approximately 10 min. • The developed method had a working range of 0.5 to 40 μmol L{sup −1} and a detection limit of 0.3 μmol L{sup −1}.

  5. Determination of the thermodynamic quantities of complexation between Eu(III) and carboxylic acids by microcalorimetry

    International Nuclear Information System (INIS)

    Potentiometric and microcalorimetric titration techniques were applied to determine the Gibbs free energies and enthalpies of the protonation of some carboxylic acids (acetic, glycolic, malonic and malic acids) and their complexation with Eu(III) in 1.0 M NaClO4 solution at 25 C, where Eu(III) was used as a chemical analogue of radiologically important Am(III). By using the values of ΔG determined by potentiometric titrations, the results of calorimetric titrations were analyzed to give the values of ΔH and ΔS. To support the discussion on the obtained thermodynamic quantities, the hydration numbers of Eu(III) in the complexes were obtained by TRLFS measurement, where the luminescence lifetime of Eu(III) excited by 394 nm laser was measured. A few to several kJ/mol of enthalpies were determined for the reactions within the uncertainties of ±0.01 to ±0.4. These enthalpy values indicated that the protonation of these carboxylates were entropy-driven, that is, vertical stroke - TΔS vertical stroke >> vertical stroke ΔH vertical stroke in ΔG = ΔH - TΔS. The complexations of Eu(III) were also shown to be controlled mainly by entropy term. The results of TRLFS measurement revealed that the number of dehydrated water molecule increased with the degree of complexation. A linear relation was found between total entropy change of the system (ΔST) and the net number of released molecules from the central Eu(III) ion. However, the values of ΔST for the hydroxy-carboxylates were smaller than that for simple carboxylates at the same net number of molecules released from Eu(III), suggesting that the dehydration occurred not only in the cation but also in the anion. (orig.)

  6. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  7. Determination of Nitric Acid in Aqueous Solution of Uranium and Plutonium Purification Cycle by Near Infrared Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    LI; Ding-ming; WANG; Lin; ZHANG; Li-hua; GONG; Yan-ping; MU; Ling; WU; Ji-zong

    2012-01-01

    <正>The concentration of nitric acid interfered with the distribution of uranium and plutonium in nuclear fuel reprocessing process. So, in the reprocessing process control analysis, the determination of the free acid plays an important role. Traditional laboratory analytical method of free acid needs large size sample and is time-consuming. Hence, development of fast analytical method for free acid has important significance for the reprocessing process control analysis. Near-infrared spectroscopy (NIRS) has been proved to be a powerful analytical tool and used in various fields, it’s seldom, however, used in spent

  8. SINTEZA IN KARAKTERIZACIJA NANODELCEV CdS IN CdSe S SONOKEMIJSKO METODO V VODNEM MEDIJU

    OpenAIRE

    Danč, Valerija

    2010-01-01

    Sonokemija je področje kemije, kjer na potek kemijskih reakcij odločilno vpliva zvočna energija v obliki ultrazvoka. Ultrazvok in z njimi povezani pojavi so že znani več kot sto let, njegova uporaba v kemiji pa dosega razcvet v današnjem času. Naše raziskave so temeljile na sintezah nanodelcev kadmijevih sulfidov (CdS) in kadmijevih selenidov (CdSe) s sonokemijsko metodo. Ta metoda se je pri sintezah pokazala kot zelo uporabna, saj so končni produkti nanokristalinični materiali. Namen ra...

  9. Determination of ethanol in acetic acid-containing samples by a biosensor based on immobilized Gluconobacter cells

    Directory of Open Access Journals (Sweden)

    VALENTINA A. KRATASYUK

    2012-11-01

    Full Text Available Reshetilov AN, Kitova AE, Arkhipova AV, Kratasyuk VA, Rai MK. 2012. Determination of ethanol in acetic acid containing samples by a biosensor based on immobilized Gluconobacter cells. Nusantara Bioscience 4: 97-100. A biosensor based on Gluconobacter oxydans VKM B-1280 bacteria was used for detection of ethanol in the presence of acetic acid. It was assumed that this assay could be useful for controlling acetic acid production from ethanol and determining the final stage of the fermentation process. Measurements were made using a Clark electrode-based amperometric biosensor. The effect of pH of the medium on the sensor signal and the analytical parameters of the sensor (detection range, sensitivity were investigated. The residual content of ethanol in acetic acid samples was analyzed. The results of the study are important for monitoring the acetic acid production process, as they represent a method of tracking its stages

  10. O-Anisidine as Indicator in Titrimetric Determination of Ascorbic Acid and Isonicotinic Acid Hydrazide in Pharmaceutical Formulations

    OpenAIRE

    Andrews, B. S. A.; B.Sreenivas Rao; Som Shankar Dubey; B.Venkata Kiran

    2010-01-01

    Inspite of the beautiful red coloured oxidized product of O-anisidine, the studies on its application in analytical techniques are scanty. So, authors have taken up the investigation on the utility of O-anisidine as a new Analytical reagent in the bromatometric-Indicator reaction. The detailed reaction on the potassium bromate and OAnisidine has enabled the authors to utilize O-Anisidine in titration of Ascorbic Acid and Isonicitonic Acid Hydrazide. Suitable conditions has been established wi...

  11. Fourier Transform Infrared (FTIR) Spectroscopy as a Utilitarian Tool for the Routine Determination of Acidity in Ester-Based Oils.

    Science.gov (United States)

    Meng, Xianghe; Li, Lei; Ye, Qin; van de Voort, Frederik

    2015-09-23

    A primary Fourier transform infrared (FTIR) method capable of determining acidity in ester-based oils is described and evaluated. Absolute free fatty acid (%FFA) and acid value (AV) calibrations were devised by spiking oleic acid into a refined, acid-free oil and measuring ν COO(-) at ∼ 1569 and ν phenolate(-) at ∼ 1588 cm(-1), respectively, in the second-derivative differential spectra. The FTIR acidity predictions were compared to the AOCS titrimetric method using acid mixtures as well as acid containing used vendor oils of undefined makeup and provenance, using two spectroscopically divergent reference oils as AC0. Relative to the AOCS reference method, the FTIR procedure was found to be both more accurate (± 0.107 vs ± 0.122) and reproducible (± 0.025 vs ± 0.077) in determining %FFA and similar in predicting AV. The FTIR phenolate method overcomes a variety of limitations of earlier FTIR-based methods, being particularly simple and well suited to routine, semiautomated acidity analysis of ester-based oils using a basic FTIR spectrometer. PMID:26321291

  12. Determining Total Phenolics, Anthocyanin Content and Ascorbic Acid Content in Some Plum Genotypes Grown in Ardahan Ecological Conditions

    Directory of Open Access Journals (Sweden)

    Z. T. ABACI

    2014-06-01

    Full Text Available In this study, total phenol content, total anthocyanin content, brix, pH, titrable acidity and total ascorbic acid content in the five plum genotypes cultivated in Ardahan City are determined and sustenance of the plums are revealed. Total phenol content was determined with folin-ciocalteu’s method, total anthocyanin content was determined with pH differential method and total ascorbic acid was determined with 2,6-dichlorophenolindophenol method.It is detected that the genotype with the highest brix content (%13.9 and lowest acidity (%0.98 is cancur, the genotype with the lowest brix content (%11 and highest acidity (%2.06 is wild plum, the genotype with the highest content of total anthocyanin, total phenolic substance and ascorbic acid is the wild plum and the genotype with the least content of these is the water plum. As a result of the study, it is revealed that the plum fruit has high levels of phenolic substance, anthocyanin and ascorbic acid content, so it has a high sustenance.

  13. Bile acid derivatives as ligands of the farnesoid x receptor: molecular determinants for bile acid binding and receptor modulation.

    Science.gov (United States)

    Gioiello, Antimo; Cerra, Bruno; Mostarda, Serena; Guercini, Chiara; Pellicciari, Roberto; Macchiarulo, Antonio

    2014-01-01

    Bile acids are a peculiar class of steroidal compounds that never cease to amaze. From being simple detergents with a primary role in aiding the absorption of fats and fat-soluble vitamins, bile acids are now widely considered as crucial hormones endowed with genomic and non-genomic functions that are mediated by their interaction with several proteins including the nuclear receptor Farnesoid X Receptor (FXR). Taking advantages of the peculiar properties of bile acids in interacting with the FXR receptor, several biliary derivatives have been synthesized and tested as FXR ligands. The availability of these compounds has contributed to characterize the receptor from a structural, patho-physiological and therapeutic standpoint. Among these, obeticholic acid is a first-in-class FXR agonist that is demonstrating hepatoprotective effects upon FXR activation in patients with liver diseases such as primary biliary cirrhosis and nonalcoholic steatohepatitis. This review provides an historical overview of the rationale behind the discovery of obeticholic acid and chemical tools generated to depict the molecular features and bio-pharmacological relevance of the FXR receptor, as well as to summarize structure-activity relationships of bile acid-based FXR ligands so far reported. PMID:25388535

  14. Interactions of Night Blue with Nucleic Acids and Determination of Nucleic Acids Using Resonance Light Scattering Technique

    Institute of Scientific and Technical Information of China (English)

    吴会灵; 梁宏; 等

    2003-01-01

    The noncovalent interactions of night blue (NB) with several nucleic acids in buffer medium of Britton-Robinson at pH 4.1 have been studied by spectroscopic methods.It is shown that the binding of NB with nucleic acids involves the J-aggregation of NB molecules on the surface of nucleic acids.The aggregation was encouraged by polyanions nucleic acids,in which nucleic acids served for acting templates,In this connection,a new method of nucleic acids with sensitivity at nanogram level is proposed based on the measurement of enhanced resonance light scattering (RLS).The linear range of ctDNA,fsDNA and yRNA is 0.01-2.5,0.03-2.5 and 0.04-1.0 μg/mL,respectively,and the corresponding detection limits(3σ)are 9.4,7.3 and 5.7ng/mL at 2.5×1005mol/L of NB.Synthetic and real samples were analyzed with satisfactory results.

  15. Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction

    Energy Technology Data Exchange (ETDEWEB)

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz [Islamic Azad University, Department of Chemistry, Science and Research Branch, Tehran (Iran)

    2006-11-15

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 {mu}g g{sup -1} and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. (orig.)

  16. Determination of hepatic uridine 5'-diphosphoglucuronic acid concentration by conjugation with diethylstilbestrol.

    Science.gov (United States)

    Watkins, J B; Klaassen, C D

    1982-03-01

    A sensitive and reliable assay for uridine 5'-diphosphoglucuronic acid (UDPGA) was developed that involved conjugation of diethylstilbestrol (DES) in vitro. This conjugation reaction is solely dependent upon UDPGA concentration. The assay uses 0.13 M Tris-HCl, pH 7.4, 6.7 mM MgCl2, 0.05% Brig 58, 0.25 mg guinea pig liver microsomal protein, 0.13 mM 3H-DES (0.2 microCi/ml), and 200 microliters of boiled 10% liver homogenate in a total volume of 0.5 ml. After a 60-min incubation at 37 degrees C, unconjugated DES is extracted into 5 ml of chloroform and the residual metabolized 3H-DES in the aqueous phase is determined by liquid scintillation spectrometry. After addition of beta-glucuronidase to the aqueous phase, about 90% of the radioactivity could be extracted into chloroform, demonstrating the DES-glucuronic acid is the primary metabolite. Thus, this method easily permits quantitation of UDPGA in rat liver in the 1-10 nmol range.

  17. Lipid nutritional value of legumes: Evaluation of different extraction methods and determination of fatty acid composition.

    Science.gov (United States)

    Caprioli, Giovanni; Giusti, Federica; Ballini, Roberto; Sagratini, Gianni; Vila-Donat, Pilar; Vittori, Sauro; Fiorini, Dennis

    2016-02-01

    This study sought to contribute to the assessment of the nutritional properties of legumes by determining the fatty acid (FA) composition of 29 legume samples after the evaluation of nine extraction methods. The Folch method and liquid-solid extraction with hexane/isopropanol or with hexane/acetone were investigated, as was the effect of previous hydration of samples. Soxhlet extractions were also evaluated with different solvent mixtures. Results on FA composition using the hexane/isopropanol extraction method were the same in terms of FA composition of the Folch method, but the extraction yield was only around 20-40% of that of the Folch method preceded by hydration. Some types of legumes showed particularly interesting values for the ratio of polyunsaturated fatty acids (PUFAs) n-6/n-3, such as lentils, with the value of 4.0, and Azuki beans, at 3.2. In lentils, the PUFAs% ranged from 42.0% to 57.4%, while in Azuki beans it was 57.5%. PMID:26304436

  18. Spectrophotometric Determination of Gemifloxacin Mesylate, Moxifloxacin Hydrochloride, and Enrofloxacin in Pharmaceutical Formulations Using Acid Dyes

    Directory of Open Access Journals (Sweden)

    Ayman A. Gouda

    2014-01-01

    Full Text Available Simple, rapid, and extractive spectrophotometric methods were developed for the determination of some fluoroquinolones antibiotics: gemifloxacin mesylate (GMF, moxifloxacin hydrochloride (MXF, and enrofloxacin (ENF in pure forms and pharmaceutical formulations. These methods are based on the formation of ion-pair complexes between the basic drugs and acid dyes, namely, bromocresol green (BCG, bromocresol purple (BCP, bromophenol blue (BPB, bromothymol blue (BTB, and methyl orange (MO in acidic buffer solutions. The formed complexes were extracted with chloroform and measured at 420, 408, 416, 415, and 422 nm for BCG, BCP, BPB, BTB, and MO, respectively, for GMF; at 410, 415, 416, and 420 nm for BCP, BTB, BPB, and MO, respectively, for MXF; and at 419 and 414 nm for BCG and BTB, respectively, in case of ENF. The analytical parameters and their effects are investigated. Beer’s law was obeyed in the ranges 1.0–30, 1.0–20, and 2.0–24 μg mL−1 for GMF, MXF, and ENF, respectively. The proposed methods have been applied successfully for the analysis of the studied drugs in pure forms and pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and indicated no significant difference in accuracy and precision.

  19. Determination of tartaric acid in wines by FIA with tubular tartrate-selective electrodes.

    Science.gov (United States)

    Sales, M G; Amaral, C E; Matos, C M

    2001-03-01

    A flow injection analysis (FIA) system comprising a tartrate-(TAT) selective electrode has been developed for determination of tartaric acid in wines. Several electrodes constructed for this purpose had a PVC membrane with a complex of quaternary ammonium and TAT as anion exchanger, a phenol derivative as additive, and a more or less polar mediator solvent. Characterization of the electrodes showed behavior was best for membranes with o-nitrophenyl octyl ether as solvent. On injection of 500 microL into a phosphate buffer carrier (pH = 3.1; ionic strength 10(-2) mol/L) flowing at 3 mL/min, the slope was 58.06 +/- 0.6 with a lower limit of linear range of 5.0 x 10(-4) mol/L TAT and R2 = 0.9989. The interference of several species, e.g. chloride, bromide, iodide, nitrate, gallic acid, tannin, sucrose, glucose, fructose, acetate, and citrate, was evaluated in terms of potentiometric selectivity coefficients. The Hofmeister series was followed for inorganic species and the most interfering organic ion was citrate. When red and white wines were analyzed and the results compared with those from an independent method they were found to be accurate, with relative standard deviations below 5.0%.

  20. Extraction concentration and atomic emission determination of controlled elements in acid mine waters

    Energy Technology Data Exchange (ETDEWEB)

    Petrov, B.I.; Oshchepkova, A.P. (Permskij Gosudarstvennyj Univ. (USSR))

    1984-09-01

    Exchange reactions between metal (Cd, Zn, Co, Hg, etc.) dithizonates and diantipyrylmethane (DAM) salts in non-aqueous solutions have been examined. Metal ions forming stable thiocyanate or iodide complexes (Cd(SCN)/sub 4//sup 2 -/, CdI/sub 4//sup 2 -/) pass from the dithizonates to form anionic complexes and then ion pairs with protonated DAM. Addition of DAM salts to organic extracts is an effective method of decomposition of dithizonates and preconcentration of elements in a microphase formed due to extract separation into two phases. A combination of preconcentration of microelements in a three-phase system with atomic emission analysis makes it possible to determine a group of controlled micro elements in complex acid mine waters.

  1. Determination of acidic isoferritin and ferritin in the serum and cancer tissues of lung cancer patients

    International Nuclear Information System (INIS)

    The serum AIF (acidic isoferritin) and Ferr (ferritin) levels are determined for 16 patients with pulmonary tuberculosis, 24 patients with pneumonia, 34 patients with lung cancer and 95 normal donors with RIA method. The results are 142.2 +- 84.5 μg/l and 104.2 +- 59.3 mg/l, 148.8 +- 79.5 μg/l and 107.3 +- 46.8 mg/l, 260.7 +- 126.3 μg/l and 161.5 +- 75.3 mg/l, and 103.8 +- 54.3 μg/l and 72.1 +- 39.5 mg/l, respectively. The lung cancer patients group has a remarkably high level as compared with other groups (P<0.01), which indicates that the serum AIF and Ferr contents can be used as important indices in lung cancer diagnosis

  2. Electrochemical Determination of Glycoalkaloids Using a Carbon Nanotubes-Phenylboronic Acid Modified Glassy Carbon Electrode

    Science.gov (United States)

    Wang, Huiying; Liu, Mingyue; Hu, Xinxi; Li, Mei; Xiong, Xingyao

    2013-01-01

    A versatile strategy for electrochemical determination of glycoalkaloids (GAs) was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA) modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors. PMID:24287539

  3. Electrochemical Determination of Glycoalkaloids Using a Carbon Nanotubes-Phenylboronic Acid Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Huiying Wang

    2013-11-01

    Full Text Available A versatile strategy for electrochemical determination of glycoalkaloids (GAs was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors.

  4. Determination of a novel bile acid sequestrant in rodent diet by near-infrared spectroscopy.

    Science.gov (United States)

    Scull, J R; Moyer, K L; Green, J S; Woodeshick, R W; Alasandro, M S

    1999-05-01

    DMP 504 is a high molecular weight polymer currently under development by The DuPont Merck Pharmaceutical Company as a novel bile acid sequestrant to lower serum cholesterol. To assess its safety, DMP 504 is incorporated into rodent diet for oral administration to rats and mice. An analytical method was developed to determine the accuracy and homogeneity of the blends. Since a physical separation or extraction of DMP 504 from the diet was not feasible, near-infrared spectroscopy (near-IR) was employed. The near-IR method provides accurate and precise results for blends containing 1.5-8.0% of DMP 504. Comparison of results at the 1.5% level with a cholate binding referee method is also presented. Both methods provided equivalent results for the 1.5% level.

  5. Determination of hydroxyl radicals with salicylic acid in aqueous nitrate and nitrite solutions

    Institute of Scientific and Technical Information of China (English)

    YANG Xi; ZHAN Man-jun; KONG Ling-ren; WANG Lian-sheng

    2004-01-01

    The qualitative and quantitative analyses of reactive oxygen species are essential to determine their steady-state concentration and related reaction mechanisms in environmental aquatic systems. In this study, salicylic acid was employed as an innovative molecular probe of hydroxyl radical(OH) generated in aqueous nitrate and nitrite solutions through photochemical reactions. Kinetic studies showed that the steady-state concentrations of OH in aqueous NO3-(10 mmol/L, pH = 5) and NO2- (10 mmol/L, pH = 5) solutions under ultraviolet irradiation were at a same magnitude, 10-15 mol/L. Apparent quantum yields of OH at 313 nm were measured as 0.011 and 0.07 for NO3- and NO2- respectively, all comparable to the results of previous studies.

  6. Determination of organic acids evolution during apple cider fermentation using an improved HPLC analysis method

    NARCIS (Netherlands)

    Zhang, H.; Zhou, F.; Ji, B.; Nout, M.J.R.; Fang, Q.; Zhang, Z.

    2008-01-01

    An efficient method for analyzing ten organic acids in food, namely citric, pyruvic, malic, lactic, succinic, formic, acetic, adipic, propionic and butyric acids, using HPLC was developed. Boric acid was added into the mobile phase to separate lactic and succinic acids, and a post-column buffer solu

  7. RP-HPLC Determination and Pharmacokinetic Comparison of Cinnamic Acid in Rat Plasma After Administration of Di-Gu-Pi Decoction and Pure Cinnamic Acid

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    A sensitive, simple, and accurate method was developed for the determination and pharmacokinetic comparison of cinnamic acid in rat plasma after the administration of a Traditional Chinese Medicinal preparation, Di-Gu-Pi decoction, and pure cinnamic acid using RP-HPLC. Di-Gu-Pi was extracted with 5% aqueous sodium bicarbonate, which was followed by purification with ion exchange column chromatography. The plasma samples taken from rats were deproteinized with methanol. The reversed-phase(HPLC) system with a Diamonsil C18 column and methanol-acetonitrile-water (8∶32∶60, volume ratio) (adjusted to pH=3.0 with glacial acetic acid) as the mobile phase was employed for the separation of cinnamic acid in the plasma samples. The detection was set at 272 nm and 3-(p-fluorophenyl)-2-propenoic acid was chosen as the internal standard. The calibration curve was linear in a range from 0.10 to 25.0 μg/mL (R2=0.9988, n=9). The precision was 3.42%-10.10%; the between-day precision was 2.84%-8.91%; the accuracy was -1.51%-1.26%; the mean recovery was 99.9%. The method was found to be sensitive, simple, accurate and appropriate for the determination of cinnamic acid.

  8. Mercaptopropionic acid-capped CdTe quantum dots as fluorescence probe for the determination of salicylic acid in pharmaceutical products.

    Science.gov (United States)

    Bunkoed, Opas; Kanatharana, Proespichaya

    2015-11-01

    Mercaptopropionic acid (MPA)-capped cadmium telluride (CdTe) quantum dot (QDs) fluorescent probes were synthesized in aqueous solution and used for the determination of salicylic acid. The interaction between the MPA-capped CdTe QDs and salicylic acid was studied using fluorescence spectroscopy and some parameters that could modify the fluorescence were investigated to optimize the measurements. Under optimum conditions, the quenched fluorescence intensity of MPA-capped CdTe QDs was linearly proportional to the concentration of salicylic acid in the range of 0.5-40 µg mL(-1) with a coefficient of determination of 0.998, and the limit of detection was 0.15 µg mL(-1). The method was successfully applied to the determination of salicylic acid in pharmaceutical products, and satisfactory results were obtained that were in agreement with both the high pressure liquid chromatography (HPLC) method and the claimed values. The recovery of the method was in the range 99 ± 3% to 105 ± 9%. The proposed method is simple, rapid, cost effective, highly sensitivity and eminently suitable for the quality control of pharmaceutical preparation. The possible mechanisms for the observed quenching reaction was also discussed.

  9. Identification of Novel Genetic Determinants of Erythrocyte Membrane Fatty Acid Composition among Greenlanders.

    Directory of Open Access Journals (Sweden)

    Mette Korre Andersen

    2016-06-01

    Full Text Available Fatty acids (FAs are involved in cellular processes important for normal body function, and perturbation of FA balance has been linked to metabolic disturbances, including type 2 diabetes. An individual's level of FAs is affected by diet, lifestyle, and genetic variation. We aimed to improve the understanding of the mechanisms and pathways involved in regulation of FA tissue levels, by identifying genetic loci associated with inter-individual differences in erythrocyte membrane FA levels. We assessed the levels of 22 FAs in the phospholipid fraction of erythrocyte membranes from 2,626 Greenlanders in relation to single nucleotide polymorphisms genotyped on the MetaboChip or imputed. We identified six independent association signals. Novel loci were identified on chromosomes 5 and 11 showing strongest association with oleic acid (rs76430747 in ACSL6, beta (SE: -0.386% (0.034, p = 1.8x10-28 and docosahexaenoic acid (rs6035106 in DTD1, 0.137% (0.025, p = 6.4x10-8, respectively. For a missense variant (rs80356779 in CPT1A, we identified a number of novel FA associations, the strongest with 11-eicosenoic acid (0.473% (0.035, p = 2.6x10-38, and for variants in FADS2 (rs174570, LPCAT3 (rs2110073, and CERS4 (rs11881630 we replicated known FA associations. Moreover, we observed metabolic implications of the ACSL6 (rs76430747 and CPT1A (rs80356779 variants, which both were associated with altered HbA1c (0.051% (0.013, p = 5.6x10-6 and -0.034% (0.016, p = 3.1x10-4, respectively. The latter variant was also associated with reduced insulin resistance (HOMA-IR, -0.193 (0.050, p = 3.8x10-6, as well as measures of smaller body size, including weight (-2.676 kg (0.523, p = 2.4x10-7, lean mass (-1.200 kg (0.271, p = 1.7x10-6, height (-0.966 cm (0.230, p = 2.0x10-5, and BMI (-0.638 kg/m2 (0.181, p = 2.8x10-4. In conclusion, we have identified novel genetic determinants of FA composition in phospholipids in erythrocyte membranes, and have shown examples of links

  10. [Determination of organic acids and inorganic anions by gradient ion chromatography].

    Science.gov (United States)

    Liu, Z; Liu, K; Shen, D; Song, Q; Mou, S; Feng, Y

    1997-07-01

    The chromatographic conditions for separation and detection of organic acids and inorganic anions by gradient ion chromatography with suppressed conductivity detection were studied. The optimized gradient programs were established. Ion chromatography were performed with a DX-100 chromatograph (DIONEX). The separation column is IonPac-AS11. Compared with NaHCO3/Na2CO3 and Na2B4O7, NaOH was the optimal eluent. The effect of organic modifier was also studied. Among methanol, 2-propanol and acetonitrile, methanol can make ion pairs such as malate and succinate, malonate and tartrate gaining baseline resolution. By using ion exchange separation, Cl-, NO3-, malate, succinate, malonate, tartrate, SO4(2-), oxalate were eluted between 5 mmol/L NaOH-16% CH3OH and 10 mmol/L NaOH-16% CH3OH in 25 min. A mobile phase composed of 30 mmol/L NaOH, 50% CH3OH and D.I. water was chosen to elute two groups of organic acids and inorganic anions: (1) quinate, formate, Cl-, malate, malonate, oxalate, citrate, isocitrate, aconitate; (2) lactate, Cl-, SO4(2-), tartrate, PO4(3-), citrate, isocitrate, aconitate. The detection limits (S/N = 3) were 0.1625 (quinate), 0.0691 (formate), 0.0115 (Cl-), 0.0886 (malate), 0.0591 (malonate), 0.0263 (oxalate), 0.1147 (citrate), 0.2017 (isocitrate), 0.3656 (cis-aconitate), 0.1045 (trans-aconitate), 0.1950 (lactate), 0.0729 (tartrate), 0.0224 (SO4(2-)) and 0.0692 (PO4(3-)) mg/L. The relative standard deviations were lower than 11.9% (n = 7) and the correlation coefficients ranged from 0.9212 for Cl- to 0.9999 for formate. The method was applied to determine the organic acids and inorganic anions of beverages and citric acids fermenting-medium. The results were satisfactory.

  11. Determination model for cetane number of biodiesel at different fatty acid composition: a review

    Directory of Open Access Journals (Sweden)

    Michal Angelovič

    2014-05-01

    Full Text Available The most accepted definition of biodiesel is stated at the EU technical regulation EN 14214 (2008 or in the USA in ASTM 6751-02. As a result of this highly strict description only methyl esters of fatty acids conform to these definitions, nevertheless the term ‘‘biodiesel’’ is spread out to other alkyl fatty esters. Some countries have adopted bioethanol for replacement of methanol in biodiesel transesterification and thus assuring a fully biological fuel. Of course, such position brings some problems in fulfilling technical requirements of EN 14214 or ASTM 6751-02. Biodiesel is actually a less complex mixture than petrodiesel, but different feedstock origins and the effect of seasonality may impose difficulties in fuel quality control. Since biodiesel is an alternative diesel fuel derived from the transesterification of triacylglycerol comprised materials, such as vegetable oils or animal fats, with simple alcohols to furnish the corresponding mono-alkyl esters, its composition depends on the raw material used, the cultivated area location, and harvest time. The choice of the raw material is usually the most important factor for fluctuations of biodiesel composition, because different vegetable oils and animal fats may contain different types of fatty acids. Important properties of this fuel vary significantly with the composition of the mixture. Cetane number, melting point, degree of saturation, density, cloud point, pour point, viscosity, and nitrogen oxides exhaust emission (NOx, for instance, deserve to be mentioned. One of the most important fuel quality indicators is the cetane number; however its experimental determination may be an expensive and lengthy task. To weaken situation concerning biodiesel, the availability of data in the literature is also scarce. In such scenario, the use of reliable models to predict the cetane number or any other essential characteristic may be of great utility. We reviewed available literature to

  12. Fabrication and characterisation of high performance polypyrrole modified microarray sensor for ascorbic acid determination

    Energy Technology Data Exchange (ETDEWEB)

    Samseya, J. [Alagappa University, Karaikudi, Tamil Nadu (India); Srinivasan, R., E-mail: sivarunjan@gmail.com [Central Electro Chemical Research Insititute, Karaikudi, Tamil Nadu (India); Chang, Yu-Tsern; Tsao, Cheng-Wen [Department of Cosmetic Applications, Taoyuan Innovation Institute of Technology, Taiwan (China); Vasantha, V.S. [Madurai Kamaraj University, Madurai, Tamil Nadu (India)

    2013-09-02

    Graphical abstract: -- Highlights: •Gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. •Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared. •Ppy/Au/MEA used for ascorbic acid determination in the presence of different neurotransmitters. •The micro array exhibited wide linear range, very high sensitivity and very low LOD than the earlier reports. •It was used successfully to test ascorbic acid in different types real samples. -- Abstract: In this study, gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared by cyclic voltammetry technique. The deposition potential range and number of cycles were optimised in order to get optimum thickness of Ppy film. Scanning Electron Microscope and Atomic Force Microscope investigations reveal that Ppy coating formed at 3 cycles is porous with thickness of 1.5 μm which exhibiting high catalytic current for ascorbic acid (AA) in square wave technique (SWV). In contrast to earlier sensors designs, these Ppy/Au/MEA sensors exhibits lower detection limit (LOD) of 10 nm towards AA at physiological conditions. It also exhibits enhanced sensitivity (2.5 mA cm{sup −2} mM{sup −1}) and long range of linear detection limit from 10 nm to 2.8 mM. In the same way, polypyrrole modified macro Au (Ppy/Au/MA) biosensor was also fabricated and its electro catalytic property towards AA was compared with that of Ppy/Au/MEA. The Ppy/Au/MA exhibits sensitivity of only 0.27 mA cm{sup −2} mM{sup −1}, LOD of 5 μM and linear range of 10 μM to 2.2 mM. Hence, our investigations indicate that the Ppy/Au/MEA could serve as highly sensitive sensor for AA than any of the earlier designs. So, the Ppy/Au/MEA electrode was utilised for determination AA in a wide variety of real samples.

  13. Electrochemical determination of activation energies for methanol oxidation on polycrystalline platinum in acidic and alkaline electrolytes.

    Science.gov (United States)

    Cohen, Jamie L; Volpe, David J; Abruña, Héctor D

    2007-01-01

    The oxidation pathways of methanol (MeOH) have been the subject of intense research due to its possible application as a liquid fuel in polyelectrolyte membrane (PEM) fuel cells. The design of improved catalysts for MeOH oxidation requires a deep understanding of these complex oxidation pathways. This paper will provide a discussion of the literature concerning the extensive research carried out in acidic and alkaline electrolytes. It will highlight techniques that have proven useful in the determination of product ratios, analysis of surface poisoning, anion adsorption, and oxide formation processes, in addition to the effects of temperature on the MeOH oxidation pathways at bulk polycrystalline platinum (Pt(poly)) electrodes. This discussion will provide a framework with which to begin the analysis of activation energy (E(a)) values. This kinetic parameter may prove useful in characterizing the rate-limiting step of the MeOH oxidation at an electrode surface. This paper will present a procedure for the determination of E(a) values for MeOH oxidation at a Pt(poly) electrode in acidic and alkaline media. Values from 24-76 kJ mol(-1) in acidic media and from 36-86 kJ mol(-1) in alkaline media were calculated and found to be a function of applied potential and direction of the potential sweep in a voltammetric experiment. Factors that influence the magnitude of the calculated E(a) include surface poisoning from MeOH oxidation intermediates, anion adsorption from the electrolyte, pH effects, and oxide formation processes. These factors are all potential, and temperature, dependent and must clearly be addressed when citing E(a) values in the literature. Comparison of E(a) values must be between systems of comparable electrochemical environment and at the same potential. E(a) values obtained on bulk Pt(poly), compared with other catalysts, may give insight into the superiority of other Pt-based catalysts for MeOH oxidation and lead to the development of new catalysts

  14. Determination of stearic acid in foodstuffs%食品中硬脂酸的测定

    Institute of Scientific and Technical Information of China (English)

    吴云辉; 理云露; 徐敦明

    2014-01-01

    目的:建立两种食品中硬脂酸含量测定的方法,以了解食品中硬脂酸的含量,并对两种测定方法进行比较。方法样品经提取脂肪后进行甲酯化衍生,采用气相色谱法(GC)和气相色谱串联质谱法(GC-MS)进行定量分析。结果 GC法和GC-MS法分别在5~500 mg/L和0.05~1 mg/mL范围内线性良好,相关系数R2大于0.99。GC法通过扣除本底值的方法,在1.0、1.2和1.5 mg/kg三个添加浓度上回收率范围为77.6%~93.8%,相对标准偏差小于12%,方法检出限和定量限分别为3.3 mg/kg和10.0 mg/kg。GC-MS法在0.2、0.25和0.3 mg/kg三个添加浓度上回收率范围为83.8%~102.9%,相对标准偏差小于10%,方法检出限和定量限分别为0.06 mg/kg和0.2 mg/kg。两方法测定的结果经计算线性回归,相关系数为0.9949,两结果不存在显著差异。结论两种方法重复性好,灵敏度满足国内外对食品中硬脂酸的检测要求,可用于大量样品的定量分析。%Objective Two methods for the determination of stearic acid were developed in order to realize the content of stearic acid in foodstuffs.Methods Samples were determined by Gas Chromatography and Gas Chromatography-Mass Spectrometry after extracting the fat and methyl esterfying.Results The method of GC showed the recoveries of stearic acid were between 77.6% and 93.8% with the relative standard deviations (RSDs) less than 12% at three spiked levels of 1.0, 1.2 and 1.5 mg/kg. The limit of detection (LOD) and the limit of quantification (LOQ) were 3.3 mg/kg and 10.0 mg/kg respectively. The method of GC-MS showed the recoveries of stearic acid were between 83.8% and 102.9% with RSDs less than 10% at three spiked levels of 0.2, 0.25 and 0.3 mg/kg. The LOD and the LOQ were 0.06 mg/kg and 0.2 mg/kg. The correlation coefficient was 0.9949 through regression test to the results of the two methods. Therefore, there was no significant difference between the two results.Conclusion The repeatability and

  15. Determination of tolerable fatty acids and cholera toxin concentrations using human intestinal epithelial cells and BALB/c mouse macrophages.

    Science.gov (United States)

    Tamari, Farshad; Tychowski, Joanna; Lorentzen, Laura

    2013-01-01

    The positive role of fatty acids in the prevention and alleviation of non-human and human diseases have been and continue to be extensively documented. These roles include influences on infectious and non-infectious diseases including prevention of inflammation as well as mucosal immunity to infectious diseases. Cholera is an acute intestinal illness caused by the bacterium Vibrio cholerae. It occurs in developing nations and if left untreated, can result in death. While vaccines for cholera exist, they are not always effective and other preventative methods are needed. We set out to determine tolerable concentrations of three fatty acids (oleic, linoleic and linolenic acids) and cholera toxin using mouse BALB/C macrophages and human intestinal epithelial cells, respectively. We solubilized the above fatty acids and used cell proliferation assays to determine the concentration ranges and specific concentrations of the fatty acids that are not detrimental to human intestinal epithelial cell viability. We solubilized cholera toxin and used it in an assay to determine the concentration ranges and specific concentrations of cholera toxin that do not statistically decrease cell viability in BALB/C macrophages. We found the optimum fatty acid concentrations to be between 1-5 ng/μl, and that for cholera toxin to be < 30 ng per treatment. This data may aid future studies that aim to find a protective mucosal role for fatty acids in prevention or alleviation of cholera infections. PMID:23748896

  16. Quantitative Determination of Fatty Acids in Marine Fish and Shellfish from Warm Water of Straits of Malacca for Nutraceutical Purposes

    Directory of Open Access Journals (Sweden)

    Nurnadia Abd Aziz

    2013-01-01

    Full Text Available This study was conducted to quantitatively determine the fatty acid contents of 20 species of marine fish and four species of shellfish from Straits of Malacca. Most samples contained fairly high amounts of polyunsaturated fatty acids (PUFAs, especially alpha-linolenic acid (ALA, C18:3 n3, eicosapentaenoic acid (EPA, C20:5 n3, and docosahexaenoic acid (DHA, C22:6 n3. Longtail shad, yellowstripe scad, and moonfish contained significantly higher (P<0.05 amounts of eicosapentaenoic acid (EPA, docosahexaenoic acid (DHA, and alpha-linolenic acid (ALA, respectively. Meanwhile, fringescale sardinella, malabar red snapper, black pomfret, Japanese threadfin bream, giant seaperch, and sixbar grouper showed considerably high content (537.2–944.1 mg/100g wet sample of desirable omega-3 fatty acids. The polyunsaturated-fatty-acids/saturated-fatty-acids (P/S ratios for most samples were higher than that of Menhaden oil (P/S=0.58, a recommended PUFA supplement which may help to lower blood pressure. Yellowstripe scad (highest DHA, ω-3/ω-6=6.4, P/S=1.7, moonfish (highest ALA, ω-3/ω-6=1.9, P/S=1.0, and longtail shad (highest EPA, ω-3/ω-6=0.8, P/S=0.4 were the samples with an outstandingly desirable overall composition of fatty acids. Overall, the marine fish and shellfish from the area contained good composition of fatty acids which offer health benefits and may be used for nutraceutical purposes in the future.

  17. Evaluation of spectrophotometric and HPLC methods for shikimic acid determination in plants: models in glyphosate-resistant and -susceptible crops.

    Science.gov (United States)

    Zelaya, Ian A; Anderson, Jennifer A H; Owen, Micheal D K; Landes, Reid D

    2011-03-23

    Endogenous shikimic acid determinations are routinely used to assess the efficacy of glyphosate in plants. Numerous analytical methods exist in the public domain for the detection of shikimic acid, yet the most commonly cited comprise spectrophotometric and high-pressure liquid chromatography (HPLC) methods. This paper compares an HPLC and two spectrophotometric methods (Spec 1 and Spec 2) and assesses the effectiveness in the detection of shikimic acid in the tissues of glyphosate-treated plants. Furthermore, the study evaluates the versatility of two acid-based shikimic acid extraction methods and assesses the longevity of plant extract samples under different storage conditions. Finally, Spec 1 and Spec 2 are further characterized with respect to (1) the capacity to discern between shikimic acid and chemically related alicyclic hydroxy acids, (2) the stability of the chromophore (t1/2), (3) the detection limits, and (4) the cost and simplicity of undertaking the analytical procedure. Overall, spectrophotometric methods were more cost-effective and simpler to execute yet provided a narrower detection limit compared to HPLC. All three methods were specific to shikimic acid and detected the compound in the tissues of glyphosate-susceptible crops, increasing exponentially in concentration within 24 h of glyphosate application and plateauing at approximately 72 h. Spec 1 estimated more shikimic acid in identical plant extract samples compared to Spec 2 and, likewise, HPLC detection was more effective than spectrophotometric determinations. Given the unprecedented global adoption of glyphosate-resistant crops and concomitant use of glyphosate, an effective and accurate assessment of glyphosate efficacy is important. Endogenous shikimic acid determinations are instrumental in corroborating the efficacy of glyphosate and therefore have numerous applications in herbicide research and related areas of science as well as resolving many commercial issues as a consequence of

  18. The Montessori System of Education: An Examination of Characteristic Features Set Forth in Il Metodo Della Pedagogica Scientifica. Bulletin, 1912, No. 17. Whole Number 489

    Science.gov (United States)

    Smith, Anna Tolman

    1912-01-01

    The publication of "Il metodo della pedagogica scientifica," by Dr. Maria Montessori, docent in the University of Rome, giving a full account of the inception and development of the system of education of which she is the author and the simultaneous translation of the work into English and German are events so unusual as to challenge attention.…

  19. Identification and determination of erucic acid in infant formula using Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Sabzevari O

    2007-05-01

    Full Text Available Background: Infant formula, depending on the source, contains various fatty acids, which may possess important nutritional and biological value for infants. The presence of some of these fatty acids in infant formula, however, can be harmful and toxic for the infant. In this regard, more attention has been paid to erucic acid since its accumulation in myocardial tissues may cause damage to the heart. Therefore, a limit has been set by the Codex Alimentarius for the presence of erucic acid in infant formula (less than 1% of total fatty acids. The purpose of the present study is to investigate amount of erucic acid present in three infant formulas used predominantly in Iran. Methods: Gas chromatography (GC is a valuable method applied for the separation of fatty acids, including erucic acid, from oils and oily food. Three brands of infant formulas, namely Humana, Biomil and Multi, were analyzed by GC using a wall coated open tubular (WCOT fused silica column and flame ionization detector (FID. Heneicosanoic acid was employed as an internal standard. Results: The findings showed that Humana and Biomil infant formula samples contained 0.06% and 0.002% erucic acid (from total fatty acids, respectively, while no erucic acid was detected in the Multi infant formula samples. Conclusion: The amount of erucic acid in the studied infant formulas was far below the Codex limit of 1% total fatty acids.

  20. "Determination of mycophenolic acid in human plasma by high-performance liquid chromatography"

    Directory of Open Access Journals (Sweden)

    "Mehdi Ahadi Barzoki

    2005-05-01

    Full Text Available A simple, sensitive and reproducible HPLC method is presented for determination of mycophenolic acid(MPA in human plasma. Samples were prepared after precipitation of the plasma protein by addition of acetonitrile and naproxen was used as internal standard (I.S.. Separation was performed by reversedphase HPLC, using a Hamilton PRP-C18 Column, 51% acetonitrile and 49% potassium phosphate buffer (20 mM at pH 3.0 as mobile phase, flow rate of 1.0 ml/min, and UV detection at 215 nm. MPA and I.S. had retention times of 7.5 and 11.35 min, respectively. The method showed an acceptable linearity in the range of 0.1µg/ml-40µg/ml with r2 of .9992. The concentration of 0.1µg/ml was determined as quantification limit. Mean absolute recovery was 94.8%. The mean intra- and inter-day reproducibility of method was 4.6 and 11.4% respectively.

  1. Determination of catecholamines by ion chromatography coupled to acidic potassium permanganate chemiluminescence detection

    Institute of Scientific and Technical Information of China (English)

    Hong Wei Wu; Mei Lan Chen; Dan Shou; Yan Zhu

    2012-01-01

    A simple,fast,sensitive,highly selective and eco-friendly analytical method for the determination of catecholamines in human urine by ion chromatography (IC) with chemiluminescence (CL) detection was described in this paper.Using 12 mmoi/L H2SO4 without any organic additive as eluent,three catecholamines including epinephrine (EP),norepinephrine (NE) and dopamine (DA)were well separated on a cation-exchange column.The CL detection was based on the reaction of analytes with acidic potassium permanganate in the presence of formaldehyde as an enhancer.The absence of methanol and acetonitrile in eluent made the proposed method more sensitive and eco-friendly.Under the optimal conditions,the linear range of the proposed method was in the range of 0.02-0.5 μg/mL.The limit of detection (LOD) was in the range of 0.6 and 5.1 μg/L.The relative standard deviations (RSD) for 0.1 μg/mL mixed standard solution were in the range of 0.8-1.9% (n =11).The method has been applied to the determination of catecholamines in human urine successfully.Excellent spiked recoveries were achieved for catecholamines ranged from 91.2% to 112.7%.

  2. Glassy carbon electrodes modified with gelatin functionalized reduced graphene oxide nanosheet for determination of gallic acid

    Indian Academy of Sciences (India)

    Fereshteh Chekin; Samira Bagheri; Sharifah Bee Abd Hamid

    2015-12-01

    A simple approach for the preparation of gelatin functionalized reduced graphene oxide nanosheet (Gel-RGONS) by chemical reduction of graphene oxide (GO) using gelatin as both reducing agent and stabilizing agent in an aqueous solution was developed. The morphology and structure of the Gel-RGONS were examined by X-ray diffraction, transmission electron microscopy, ultraviolet–visible spectroscopy and Raman spectroscopy. Gelatin acted as a functionalizing reagent to guarantee good dispersibility and stability of the r in distilled water. Moreover, a new electrochemical sensor was developed based on Gel-RGONS modified glassy carbon electrode (Gel-RGONS/GCE). Gel-r exhibits excellent electrocatalytic activity to gallic acid (GA) oxidation. The experimental conditions such as pH, adsorption time and scan rate were optimized for the determination of GA. Under optimum conditions, the sensor responded linearly to GA in the concentration of 1.0 × 10−6 to 1.1 × 10−4 M with detection limit of 4.7 × 10−7 M at 3 using linear sweep voltammetry (LSV). The method has been successfully applied to the determination of GA in sample of black tea.

  3. Electrochemical determination of ascorbic acid at p-phenylenediamine film-holes modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Olana Bikila Nagasa

    2015-01-01

    Full Text Available In this work the determination of ascorbic acid (AA at glassy carbon electrode (GCE modified with a perforated film produced by reduction of diazonium generated in situ from p-phenylenediamine (PD is reported. Holes were intentionally created in the modifier film by stripping a pre-deposited gold nanoparticles. The modified electrodes were electrochemically characterized by common redox probes: hydroquinone, ferrocyanide and hexamineruthenium(III. The cyclic voltammetric and amperometric response of AA using the modified electrodes was compared with that of bare GCE. The bare GCE showed a linear response to AA in the concentration range of 5 mM to 45 mM with detection limit of 1.656 mM and the modified GCE showed a linear response to AA in the concentration range of 5 μM to 45 μM with detection limit of 0.123 μM. The effect of potential intereferents on amperometric signal of AA at the modified GCE was examined and found to be minimal. The inter-electrode reproducibility, stability, and accuracy were determined. The modified electrode showed excellent inter-electrode reproducibility, accuracy and stability. The modified electrode reported is a promising candidate for use in electroanalysis of AA.

  4. Linear sweep polarographic determination of nucleic acids using acridine orange as a bioprobe

    Directory of Open Access Journals (Sweden)

    WEI SUN

    2007-11-01

    Full Text Available The interaction of acridine orange (AO with double-stranded (ds DNA in aqueous solution was investigated by linear sweep polarography (LSP on a dropping mercury working electrode (DME. In pH 2.5 Britton–Robinson (B–R buffer solution, AO had a sensitive linear sweep polarographic reductive peak at –0.89 V (vs. SCE, which could be greatly inhibited by the addition of dsDNA, with a positive shift of the peak potential. Based on the decrease of the reductive peak current, a new quantitative electrochemical determination method for dsDNA was developed with a linear range of 2.0−20.0 mg l-1 and the linear regression equation: ΔIp” (nA = 111.90 C (mg l-1+125.32 (n = 9, γ = 0.997. The influences of commonly co-existing substances, such as metal ions, amino acid, etc., on the determination were also investigated. The method is sensitive, rapid and simple with good selectivity. The new proposed method was further applied to the detection of RNA and three synthetic samples containing dsDNA with satisfactory results. The binding number and the equilibrium constant between dsDNA and AO were calculated by an electrochemical method.

  5. Precise equilibrium structure determination of hydrazoic acid (HN{sub 3}) by millimeter-wave spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Amberger, Brent K.; Esselman, Brian J.; Woods, R. Claude; McMahon, Robert J. [Department of Chemistry, University of Wisconsin–Madison, Madison, Wisconsin 53706 (United States); Stanton, John F. [Institute for Theoretical Chemistry, Department of Chemistry, The University of Texas–Austin, Austin, Texas 78712 (United States)

    2015-09-14

    The millimeter-wave spectrum of hydrazoic acid (HN{sub 3}) was analyzed in the frequency region of 235-450 GHz. Transitions from a total of 14 isotopologues were observed and fit using the A-reduced or S-reduced Hamiltonian. Coupled-cluster calculations were performed to obtain a theoretical geometry, as well as rotation-vibration interaction corrections. These calculated vibration-rotation correction terms were applied to the experimental rotational constants to obtain mixed theoretical/experimental equilibrium rotational constants (A{sub e}, B{sub e}, and C{sub e}). These equilibrium rotational constants were then used to obtain an equilibrium (R{sub e}) structure using a least-squares fitting routine. The R{sub e} structural parameters are consistent with a previously published R{sub s} structure, largely falling within the uncertainty limits of that R{sub s} structure. The present R{sub e} geometric parameters of HN{sub 3} are determined with exceptionally high accuracy, as a consequence of the large number of isotopologues measured experimentally and the sophisticated (coupled-cluster theoretical treatment (CCSD(T))/ANO2) of the vibration-rotation interactions. The R{sub e} structure exhibits remarkable agreement with the CCSD(T)/cc-pCV5Z predicted structure, validating both the accuracy of the ab initio method and the claimed uncertainties of the theoretical/experimental structure determination.

  6. Precise equilibrium structure determination of hydrazoic acid (HN3) by millimeter-wave spectroscopy

    International Nuclear Information System (INIS)

    The millimeter-wave spectrum of hydrazoic acid (HN3) was analyzed in the frequency region of 235-450 GHz. Transitions from a total of 14 isotopologues were observed and fit using the A-reduced or S-reduced Hamiltonian. Coupled-cluster calculations were performed to obtain a theoretical geometry, as well as rotation-vibration interaction corrections. These calculated vibration-rotation correction terms were applied to the experimental rotational constants to obtain mixed theoretical/experimental equilibrium rotational constants (Ae, Be, and Ce). These equilibrium rotational constants were then used to obtain an equilibrium (Re) structure using a least-squares fitting routine. The Re structural parameters are consistent with a previously published Rs structure, largely falling within the uncertainty limits of that Rs structure. The present Re geometric parameters of HN3 are determined with exceptionally high accuracy, as a consequence of the large number of isotopologues measured experimentally and the sophisticated (coupled-cluster theoretical treatment (CCSD(T))/ANO2) of the vibration-rotation interactions. The Re structure exhibits remarkable agreement with the CCSD(T)/cc-pCV5Z predicted structure, validating both the accuracy of the ab initio method and the claimed uncertainties of the theoretical/experimental structure determination

  7. Interference-Blind Microfluidic Sensor for Ascorbic Acid Determination by UV/vis Spectroscopy

    DEFF Research Database (Denmark)

    Bi, Hongyan; Oliveira Fernandes, Ana Carolina; Cardoso, Susana;

    2016-01-01

    A microfluidic sensor is developed and targeted at specific ingredients determination in drug/food/beverage matrices. The surface of a serpentine polydimethylsiloxane (PDMS) microchannel is modified by enzyme via physisorption. When solutions containing target ingredients pass through the microfl......A microfluidic sensor is developed and targeted at specific ingredients determination in drug/food/beverage matrices. The surface of a serpentine polydimethylsiloxane (PDMS) microchannel is modified by enzyme via physisorption. When solutions containing target ingredients pass through...... the microfluidic channel, enzyme-catalyzed reaction occurs and only converts the target molecules to its products. The whole process is monitored by an end-channel UV/vis spectroscopic detection. Ascorbate oxidase and L-ascorbic acid (AA) are taken as enzyme-substrate model in this study to investigate......, specific, and accurate, and can be potentially used for fast quantification of ingredient in samples with complex matrix background. It is promising to be widely spread in food industry and quality control department...

  8. Determination of modification degree in BDDE-modified hyaluronic acid hydrogel by SEC/MS.

    Science.gov (United States)

    Yang, Biao; Guo, Xueping; Zang, Hengchang; Liu, Jianjian

    2015-10-20

    Determination of modification degree in BDDE-modified hyaluronic acid (HA) hydrogel is of particular interest. In this paper, three crosslinking parameters (degree of total modification, t-MOD; degree of cross-link modification, c-MOD; degree of pendent modification, p-MOD) are defined and determined by quantification of the modified fragments in hydrogel digestion by size exclusion chromatography combined with mass spectrometry (SEC-MS). The digestion products of a novel hyaluronidase HAase-B produced by Bacillus sp. A50 are studied and only a few modified fragments are identified by (1)H NMR and MS. As a result, Three HA hydrogels prepared in lab have different t-MOD, c-MOD and p-MOD, but the ratio of c-MOD to p-MOD result in the almost same value of 75%. Hydrogel products from Q-Med have nearly same t-MOD about 0.8% and c-MOD about 0.1%, the ratio of c-MOD to p-MOD is about 13%. Hydrogels from ANTEIS S.A all have much higher t-MOD values, the ratio of c-MOD and p-MOD is about 8%.

  9. Effect of hydrofluoric acid on acid decomposition mixtures for determining iron and other metallic elements in green vegetables

    International Nuclear Information System (INIS)

    The efficiency of acid mixtures, HNO3 - HCI04 -HF, HNO3 - HCI - HF, HNO3 - HCIO4 and HNO3 - HCI in the decomposition of four edible green vegetables, Gboma (Solanum macrocarpon), Aleefu (Amaranttius hibiridus), Shoeley (Hibiscus sabdariffa) and Ademe (Corchorus olitorius), for flame Atomic Absorption Spectrometer analysis of Fe, Mn, Mg, Cu, Zn and Ca was studied. The concentrations of Fe were higher (120.61 -710.10 mg/kg), while the values of Cu were lower (2.31 - 4.84 mg/kg) in all the samples. The values of concentration for Fe were more reproducible when HF was included in the decomposition mixtures. There were no significant differences in the concentrations of the other elements when HF was included in the acid mixture as compared to the acid mixtures without HF. Therefore, the inclusion of HF in the acid decomposition mixtures would ensure total and precise estimation of Fe in plant materials, but not critical for analysis of Mn, Mg, Cu, Zn and Ca. Performance of the decomposition procedures was verified by applying the methods to analyse Standard Reference Material IAEA-V-10 Hay Powder. (au)

  10. Polymorphism in the fatty acid desaturase genes and diet are important determinants of infant n-3 fatty acid status

    DEFF Research Database (Denmark)

    Harsløf, L.B.S.; Larsen, L.H.; Ritz, C.;

    breastfeeding was obtained by questionnaires and fish intake was assessed by 7-day pre-coded food diaries. Results: FADS-genotype, breastfeeding, and fish intake were found to explain 25% of the variation in infant RBC DHA-status (mean±SD: 6.6±1.9% of the fatty acids (FA%)). Breastfeeding was the most important......Background and objectives: Tissue docosahexaenoic acid (DHA) accretion in early infancy has been shown to be supported by the DHA-content of breast-milk and thus may decrease once complementary feeding takes over. Endogenous synthesis of DHA from alpha-linolenic acid has been shown to be very low...... and polymorphism in the genes that encodes the fatty acid desaturases (FADS) has little effect on DHA-status in adults. It is however unclear to what extent endogenous DHA-synthesis contributes to infant DHA-status. Aim: To investigate the role of diet and FADS polymorphism on DHA-status at 9 months and 3 years...

  11. NF EN 14103. July 2003. Fatty compounds derived products. Fatty acids methylic esters (FAME). Determination of the ester and methylic ester content of linoleic acid; NF EN 14103. Juillet 2003. Produits derives des corps gras. Esters methyliques d'acides gras (EMAG). Determination de la teneur en ester et en ester methylique de l'acide linolenique

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2003-07-01

    This European standard aims at determining the ester and methylic ester content of fatty acids methylic esters (FAME) used as pure bio-fuels or as constituent of a heating or diesel fuel. This method allows also to determine the methylic ester content of linoleic acid. It allows to verify that the ester content of FAMEs is greater than 90% (m/m) and that the linoleic acid content is comprised between 1% (m/m) and 15% (m/m). The method is applicable to FAMEs with methylic ester contents comprised between C14 and C24. (J.S.)

  12. Silver nanoparticles plasmon resonance-based method for the determination of uric acid in human plasma and urine samples

    International Nuclear Information System (INIS)

    We have developed a simple and sensitive colorimetric procedure for the quantification of trace amounts of uric acid. It is based on the finding that uric acid in a medium containing ammonia and sodium hydroxide at 650 C can reduce silver ions to form yellow silver nanoparticles (Ag NPs). These are stabilized in solution by using poly(vinyl alcohol) as a capping agent. The yellow color of the solution that results from the localized surface plasmon resonance of Ag NPs can be observed by the bare eye. The absorbance at 415 nm is proportional to the concentration of uric acid which therefore can be determined quantitatively. The calibration curve is linear in the concentration range from 10 to 200 nM, with a limit of detection of 3.3 nM. The method was successfully applied to the determination of uric acid in human plasma and urine samples. (author)

  13. Simultaneous determination of phenolic acids and flavonoids in Lycium barbarum Linnaeus by HPLC-DAD-ESI-MS.

    Science.gov (United States)

    Inbaraj, B Stephen; Lu, H; Kao, T H; Chen, B H

    2010-02-01

    A high-performance liquid chromatography-diode array detection-mass spectrometry method with electrospray ionization mode (HPLC-DAD-ESI-MS) was developed for simultaneous determination of phenolic acids and flavonoids in fruits of Lycium barbarum Linnaeus, a widely used traditional Chinese herb possessing vital biological activity. Both phenolic acids and flavonoids were extracted with 50% ethanol and purified using a polymeric solid phase extraction cartridge followed by HPLC-DAD-ESI-MS analysis. By employing a Vydac C18 column, a total of 52 phenolic acids and flavonoids were separated within 70min using a gradient mobile phase of 0.5% (v/v) formic acid in water and acetonitrile-water (94:6, v/v) with flow rate at 1mL/min, column temperature at 30 degrees C and detection wavelength at 280nm. Of 52 compounds, 15 phenolic acids and flavonoids were positively identified based on both absorption and mass spectra, with the remaining 37 tentatively identified by comparison of absorption spectra with reported values in the literature. Internal standards 3-hydroxybenzoic acid and hesperidin were used for quantitation of phenolic acids and flavonoids, respectively. Among the 15 positively identified compounds, quercetin-rhamno-di-hexoside was present in largest mass fraction (438.6microg/g), followed by quercetin-3-O-rutinoside (281.3microg/g), dicaffeoylquinic acid isomers (250.1microg/g), chlorogenic acid (237.0microg/g), quercetin-di-(rhamnohexoside) (117.5microg/g), quercetin-di-(rhamno)-hexoside (116.8mug/g), kaempferol-3-O-rutinoside (97.7microg/g), isorhamnetin-3-O-rutinoside (72.1microg/g), p-coumaric acid (64.0microg/g), caffeic acid (23.7microg/g) and vanillic acid (22.8microg/g). PMID:19819093

  14. Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine

    International Nuclear Information System (INIS)

    Graphical abstract: An electrochemical sensor based on PAR/EGR/GCE via a cooperation of the potentiostatic technique and cyclic voltammetry was first fabricated for the determination of CPFX with satisfied detecting result of real samples. - Highlights: • PAR/EGR composite film was prepared for the first time. • The sensor can be applied to determinate CPFX in the presence of AA, UA and DA. • The sensor indicated the feasibility in drug samples and biological media. - Abstract: A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10−8 to 1.2 × 10−4 M with a detection limit (S/N = 3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media

  15. Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xin; Wei, Youli; Ding, Yaping, E-mail: wdingyp@sina.com

    2014-07-04

    Graphical abstract: An electrochemical sensor based on PAR/EGR/GCE via a cooperation of the potentiostatic technique and cyclic voltammetry was first fabricated for the determination of CPFX with satisfied detecting result of real samples. - Highlights: • PAR/EGR composite film was prepared for the first time. • The sensor can be applied to determinate CPFX in the presence of AA, UA and DA. • The sensor indicated the feasibility in drug samples and biological media. - Abstract: A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10{sup −8} to 1.2 × 10{sup −4} M with a detection limit (S/N = 3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media.

  16. Determination of nanomolar uric and ascorbic acids using enlarged gold nanoparticles modified electrode.

    Science.gov (United States)

    Kannan, P; John, S Abraham

    2009-03-01

    Individual and simultaneous determination of 50nM uric acid (UA) and ascorbic acid (AA) using enlarged, citrate-stabilized gold nanoparticles (AuNPs) self-assembled to 2,5-dimercapto-1,3,4-thiadiazole (DMT) monolayer modified Au (Au/DMT) electrode by an amperometric method is described for the first time. Self-assembly of AuNPs on the electrode surface was confirmed by atomic force microscopy (AFM), attenuated total reflectance FT-IR and diffuse reflectance spectral measurements. The electron transfer reaction (ETR) of [Fe(CN)(6)](3-/4-) was blocked at Au/DMT electrode, whereas it was restored with a peak separation of 200mV after the attachment of AuNPs on the Au/DMT (Au/DMT/AuNPs) electrode, which was confirmed from the ETR of the [Fe(CN)(6)](3-/4-) redox couple. When the self-assembled AuNPs were enlarged by hydroxylamine seeding, the ETR of [Fe(CN)(6)](3-/4-) was improved significantly with a peak separation of 100mV. Tapping mode AFM showed that the average size of the enlarged-AuNPs (E-AuNPs) was 50-70nm. The E-AuNPs modified electrode catalyzes the oxidation of AA and UA, separates their voltammetric signals by 200mV, and has excellent sensitivity towards AA and UA with a detection limit of 50nM. The practical application of the modified electrode was demonstrated by measuring the concentration of UA in blood serum and urine. PMID:19111516

  17. Quantitative determination of urinary trichloroacetic acid as an index of trichloroethylene exposure by high performance liquid chromatography.

    Directory of Open Access Journals (Sweden)

    Ogata,Masana

    1979-12-01

    Full Text Available A high performance lipuid chromatographic method for the determination of urinary trichloroacetic acid, a metabolite of trichloroethylene, is described. A stainless steel column packed with Hitachi gel 2618 (H form was used and the mobile phase was one per cent aqueous phosphoric acid. Urine can be analyzed directly without any solvent extraction or pretreatment. The minimal detection limit was 0.5 micrograms per analysis. The present method is simple and specific, and can be performed within 10 min.

  18. Rapid and sensitive liquid chromatographic method using a conductivity detector for the determination of phytic acid in food

    OpenAIRE

    Talamond, Pascale; Gallon, Georges; Trèche, Serge

    1998-01-01

    An LC method was developed for the determination of phytic acid in food. The separation was carried out by gradient elution on an anion-exchange column using a conductivity detector. Earlier reversed-phase LC procedures for the quantitation of phytic acid usually required a prepurification step. The prepurification can be avoided by the separation method described in this paper. The method is sensitive and selective, and can be rapidly and easily performed. It is therefore suitable for routin...

  19. Determination of humic and fulvic acids in commercial solid and liquid humic products by alkaline extraction and gravimetric determination

    Science.gov (United States)

    Increased use of humic substances in agriculture has generated intense interest among producers, consumers, and regulators for an accurate and reliable method for quantification of humic (HA) and fulvic acids (FA) in raw ores and products. Here we present a thoroughly validated method, the Humic Pro...

  20. The determination of titratable acidity and total tannins in red wine

    OpenAIRE

    Rajković Miloš B.; Sredović Ivana D.

    2009-01-01

    Titration acidity and content of total tannins in mass-market red wines are analyzed in this paper. The content of total acids in wine, expressed through wine acid, was analyzed by potentiometric titration on 7.00 pH value. According to titratable acidity in analyzed wines, all wines (only) with analyzed parameters according to Regulations about wine quality. The analysis of differential potentiometric curves shows that these curves can give the answer to the question if non organic substance...

  1. Simultaneous extraction and HPLC determination of 3-indole butyric acid and 3-indole acetic acid in pea plant by using ionic liquid-modified silica as sorbent.

    Science.gov (United States)

    Sheikhian, Leila; Bina, Sedigheh

    2016-01-15

    In this study, ionic liquid-modified silica was used as sorbent for simultaneous extraction and preconcentration of 3-indole butyric acid and 3-indole acetic acid in pea plants. The effect of some parameters such as pH and ionic strength of sample solution, amount of sorbent, flow rate of aqueous sample solution and eluent solution, concentration of eluent solution, and temperature were studied for each hormone solution. Percent extraction of 3-indole butyric acid and 3-indole acetic acid was strongly affected by pH of aqueous sample solution. Ionic strength of aqueous phase and temperature showed no serious effects on extraction efficiency of studied plant hormones. Obtained breakthrough volume was 200mL for each of studied hormones. Preconcentration factor for spectroscopic and chromatographic determination of studied hormones was 100 and 4.0×10(3) respectively. Each solid sorbent phase was reusable for almost 10 times of extraction/stripping procedure. Relative standard deviations of extraction/stripping processes of 3-indole butyric acid and 3-indole acetic acid were 2.79% and 3.66% respectively. The calculated limit of detections for IBA and IAA were 9.1×10(-2)mgL(-1) and 1.6×10(-1)mgL(-1) respectively.

  2. Analysis of Reaction between α-Lipoic Acid and 2-Chloro-1-methylquinolinium Tetrafluoroborate Used as a Precolumn Derivatization Technique in Chromatographic Determination of α-Lipoic Acid

    Directory of Open Access Journals (Sweden)

    Magdalena Godlewska

    2015-01-01

    Full Text Available The present study offers results of analysis concerning the course of reaction between reduced α-lipoic acid (LA and 2-chloro-1-methylquinolinium tetrafluoroborate (CMQT. In water environments, the reaction between CMQT and hydrophilic thiols proceeds very rapidly and the resultant products are stable. For the described analysis, optimum reaction conditions, such as concentration of the reducing agent, environment pH, and concentration of the reagent were carefully selected. The spectrophotometric assay was carried out measuring absorbance at λ=348 nm (i.e., the spectral band of the obtained reaction product. Furthermore, the calibration curve of lipoic acid was registered. It was concluded that the Lambert-Beer law was observed within the range 1–10 μmol L−1. Later, the reaction between LA and CMQT was used as precolumn derivatization in a chromatographic determination of the lipoic acid in the range 2.5–50 μmol L−1. Practical applicability of the designed methods was evaluated by determining lipoic acid in Revitanerv pharmaceutical preparation which contains 300 mg LA in a single capsule. The error of the determination did not exceed 0.5% in relation to the declared value.

  3. Determination of Fatty Acid Composition on Different False Flax (Camelina sativa (L.) Crantz) Genotypes under Ankara Ecological Conditions

    OpenAIRE

    KATAR, Duran

    2013-01-01

    This research was conducted to determine fatty acid composition of different false flax (Camelina sativa (L.) Crantz) genotypes (Vinimik 17, PI 304269, CR 476/65, CR 1674/90, Ames26665, Ames26667, Ames26673, Ames26676, Ames26680, Ames26686 and Ames28372) in terms of oleic, linoleic, linolenic, steraic, eicosenoic and erucic acids in 2010 and 2011. Results showed that having highest linolenic acid content, Ames28372 could be suggested to be used as oil crops for oil industry or as medicine pla...

  4. Selective Voltammetric Determination of Uric Acid in the Presence of Ascorbic Acid at Ordered Mesoporous Carbon Modified Electrodes

    Institute of Scientific and Technical Information of China (English)

    WEN,Yan-Li; JIA,Neng-Qin; WANG,Zhi-Yong; SHEN,He-Bai

    2008-01-01

    A novel chemically modified electrode was fabricated by immobilizing ordered mesoporous carbon (OMC)onto a glassy carbon (GC) electrode.The electrocatalytic behavior of the OMC modified electrode towards the oxidation of uric acid (UA) and ascorbic acid (AA) was studied.Compared to a glassy carbon electrode,the OMC modified electrode showed a faster electron transfer rate and reduced the overpotentials greatly.Furthermore,the OMC modified electrode resolved the overlapping voltammetric responses of UA and AA into two well-defined voltammetric peaks with peak separation of ca.0.38 V.All results show that the OMC modified electrode has a good electrocatalytic ability to UA and AA,and has an excellent response towards UA even in the presence of high concentration AA.

  5. Validation of a method by gas chromatography for the determination of fatty acids that comprise the active ingredient D-004

    International Nuclear Information System (INIS)

    D-004 is a new active ingredient obtained from the Cuban royal palm (Roystonea regia) fruits. This substance is mainly composed by a mixture of saturated and unsaturated free fatty acids, from 8 to 18 carbon atoms, and has shown to be effective in experimental model of prostate hyperplasia. A capillary gas chromatographic method for the determination of the fatty acids in D-004 was developed and validated. The acids were analyzed as methyl ester derivatives, which were obtained by reaction with 10 % acetyl chloride in methanol and separated in a BPX-5 wide-bore column using tridecanoic acid as internal standard. The specificity study showed no interferences regarding the determination of this mixture, once the samples were submitted to stress conditions. Determination of the total fatty acid content was linear (r > 0.999; CVs of the response factors and of the slopes lower than 5 and 2 %, respectively) and without bias in the studied concentration range, from 50 to 150 % of the nominal mass. In the accuracy study, over the range 80 to 120 % of the nominal fatty acid concentration, high recoveries (100.4 to 100.8 %) were reached. Good results were obtained in the repeatability and intermediate precision studies (CV < 2%), proving that the method is precise. These results support that this method is properly validated, being appropriate for the quality control and stability studies of this active ingredient

  6. Direct determination of seleno-amino acids in biological tissues by anion-exchange separation and electrochemical detection.

    Science.gov (United States)

    Cavalli, S; Cardellicchio, N

    1995-07-01

    Several studies have described the determination of selenium in protein extracts from tissues of marine or terrestrial animals, but have not identified the different chemical forms of selenium that are present. Selenium may be present as seleno-amino acids. Selenocysteine, for example, is a normal component of glutathione peroxidase, an antioxidant enzyme which may behave like other antioxidants, such as vitamin E, protecting tissues against methylmercury toxicity. The present study illustrates a method for the characterization of seleno-amino acids, such as selenocysteine and selenomethionine, in proteins extracted from the liver of marine mammals. The mechanism of detoxification of methylmercury, which involves seleno-compounds, is identified. The analytical determination was carried out using high-performance anion-exchange chromatography coupled with integrated pulsed amperometric detection (HPAEC-IPAD). This method allows the direct determination of underivatized amino acids, eliminating the procedure of pre- or postcolumn derivatization. The chromatographic separation was carried out on an anion-exchange column using a quaternary gradient elution. In order to optimize this method, interferences of amino acids and the influence of pH and ionic strength on the separation and electrochemical detection were studied. The IPAD response for the direct detection of amino acids is optimum at pH > 11. The detection limit (S/N = 3) for selenocysteine was found to be 450 micrograms/l. The application of this method for the identification of seleno-amino acids in protein hydrolysates is also shown. PMID:7640774

  7. Flow—injection Chemiluminescence Sensor for the Determination of Gallic Acid by Immobilizing Luminol and Periodate on Anionexchange Resin

    Institute of Scientific and Technical Information of China (English)

    鞠Huang先; 张四纯; 周国俊

    2002-01-01

    A novel chemiluminescence (CL) sensor for the determination of gallic acld combined with folw injection analysis was developed by electrostatically immobilizing hminol and periodate on anion-exchange resins respectively.Gallic acid was sensed by its enhancing effect on the weak CL reaction between luminol and periodate,which were eluted from the ion exchange column.The possible reaction mechanism of the CL system was suggested and discussed.The response of the sensor to gallic acid concentration was linear over the range of 8.0×10-—1.0×10-6mol/L with a detection limit of 6.5×10-9 mol/L(3σ).The relative standard deviation (RSD) for 7 repetitive determinations of gallic acid(1.0×10-7mol/L) was 1.8?The sensor could be used for over 400 times determination with a good reproducibility.

  8. Study and Elimination of the Interference of Aluminium on the Voltammetric Determination of Uranium with Chloranilic Acid. Application to the Determination of Uranium in Waters and Geological Samples

    International Nuclear Information System (INIS)

    The interference of aluminium during the voltammetric determination of uranium with 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone (chloranilic acid) has been investigated. The presence of aluminium originates a voltammetric signal due to its chloranilic acid complex at the same potential range as the uranium analytical signal appears. The interference of aluminium can be overcome by addition of an appropriate amount of sodium fluoride as complexing reagent. The determination of uranium by adsorptive stripping voltammetry (AdSV) can be carried out at concentration levels as low as 1 μg/L in the presence of 100 μg/L aluminium after the addition of 100μL of 0.1 mol/L NaF. The method can be applied to the determination of uranium in aluminium-containing waters and geological samples containing high aluminium levels. (Author) 19 refs

  9. Determination of Acid Herbicides Using Modified QuEChERS with Fast Switching ESI(+)/ESI(-) LC-MS/MS.

    Science.gov (United States)

    Sack, Chris; Vonderbrink, John; Smoker, Michael; Smith, Robert E

    2015-11-01

    A method for the determination of 35 acid herbicides in food matrices was developed, validated, and implemented. It utilizes a modified QuEChERS extraction procedure coupled with quantitation by liquid chromatography tandem mass spectrometry (LC-MS/MS). The acid herbicides analyzed are all organic carboxylic acids, including the older chlorophenoxy acid herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D), dicamba, 4-chlorophenoxyacetic acid (4-CPA), quinclorac, and many of the newer imidazolinone herbicides such as imazethapyr and imazaquin. In the procedure, 10 mL of water is added to 5 g of sample and then extracted with 1% formic acid in acetonitrile for 1 min. The acetonitrile phase is salted out of the extract by adding sodium chloride and magnesium sulfate, followed by centrifugation. The acetonitrile is diluted 1:1 with water to enable quantitation by LC-MS/MS using fast switching between positive and negative electrospray ionization modes. The average recoveries for all the compounds except aminocyclopyrachlor were 95% with a precision of 8%. The method detection limits for all residues were less than 10 ng/g, and the correlation coefficients for the calibration curves was greater than 0.99 for all but two compounds tested. The method was used successfully for the quantitation of acid herbicides in the FDA's total diet study. The procedure proved to be accurate, precise, linear, sensitive, and rugged. PMID:26473587

  10. Determination of total L-Ascorbic Acid by high performance liquid chromatography in human plasma

    Directory of Open Access Journals (Sweden)

    Oveisi MR

    2001-07-01

    Full Text Available The total vitamin C content in human plasma is widely accepted as an indicator of the tissue status of vitamin C. A liquid chromatography method with ultraviolet detector (264 nm for measuring ascorbic acid in human plasma was developed. A C18 reversed-phase column and cetrimide as an ion-pairing agent was employed. Ascorbic acid (AA was measured after reducing L-dehydroascorbic acid to L-ascorbic acid with dithiothreitol. The stability of the ascorbic acid in plasma, metaphosphoric acid and trichloroacetic acid was also evaluated. The analytical parameters, including linearity (1-60 µg/ml, accuracy (98.98%, repeatability (2.8% and reproducibility (7.2%, showed that the method is reliable for measuring the total vitamin C content in plasma.

  11. Determination of gadolinium and yttrium using ionic associates with 3,5-diiodo-salicylic acid and rhodamine C

    International Nuclear Information System (INIS)

    Influence of non-colored complexing substances on extraction of Gd and Y ionic associates with 3.5-diodo-saliculic acid and rhodamine B is investigated. The technique of analysis of the Gd and Y oxide mixture is developed with the use of 1.10-phenanthroline and mandelic acid asmasking reagents, first of which in the most part masks the Gd reaction, the second reagent masks the Y one. The low boundary of the determined contents constitutes 1-2%. The equilibrium constants of the substitution reaction of the rhodamine B in the 1.10-phenanthroline compounds are determined

  12. Solution of rocks and refractory minerals by acids at high temperatures and pressures. Determination of silica after decomposition with hydrofluoric acid

    Science.gov (United States)

    May, I.; Rowe, J.J.

    1965-01-01

    A modified Morey bomb was designed which contains a removable nichromecased 3.5-ml platinium crucible. This bomb is particularly useful for decompositions of refractory samples for micro- and semimicro-analysis. Temperatures of 400-450?? and pressures estimated as great as 6000 p.s.i. were maintained in the bomb for periods as long as 24 h. Complete decompositions of rocks, garnet, beryl, chrysoberyl, phenacite, sapphirine, and kyanite were obtained with hydrofluoric acid or a mixture of hydrofluoric and sulfuric acids; the decomposition of chrome refractory was made with hydrochloric acid. Aluminum-rich samples formed difficultly soluble aluminum fluoride precipitates. Because no volatilization losses occur, silica can be determined on sample solutions by a molybdenum-blue procedure using aluminum(III) to complex interfering fluoride. ?? 1965.

  13. Microemulsion electrokinetic chromatography as a suitable tool for lipophilicity determination of acidic, neutral, and basic compounds.

    Science.gov (United States)

    Subirats, Xavier; Yuan, Hui-Ping; Chaves, Verónica; Marzal, Núria; Rosés, Martí

    2016-07-01

    In the present work, several MEEKC systems are studied to assess their suitability for lipophilicity determination of acidic, neutral, and basic compounds. Thus, several microemulsion compositions over a wide range of pH values (from 2.0 to 12.0), containing heptane, 1-butanol and different types and amounts of surfactant (SDS or sodium cholate: from 1.3 to 3.3%) are characterized using Abraham's solvation model. The addition of acetonitrile (up to 10%) is also studied, since it increases the resolution of the technique for the most lipophilic compounds. The system coefficients obtained are very similar to those of the 1-octanol/water, used as the reference lipophilicity index, allowing simple and linear correlations between the 1-octanol/water partition values (log Po/w ) and MEEKC mass distribution ratios (log kMEEKC ). Variations in the microemulsion composition (aqueous buffer, surfactant, concentration of ACN) did not significantly affect the similarity of the MEEKC systems to log Po/w partition. PMID:27126602

  14. Determination of phosphate in natural waters by activation analysis of tungstophosphoric acid

    Science.gov (United States)

    Allen, Herbert E.; Hahn, Richard B.

    1969-01-01

    Activation analysis may be used to determine quantitatively traces of phosphate in natural waters. Methods based on the reaction 31P(n,γ)32P are subject to interference by sulfur and chlorine which give rise to 32P through n,p and n,α reactions. If the ratio of phosphorus to sulfur or chlorine is small, as it is in most natural waters, accurate analyses by these methods are difficult to achieve. In the activation analysis method, molybdate and tungstate ions are added to samples containing phosphate ion to form tungstomolybdophosphoric acid. The complex is extracted with 2,6-dimethyl-4-heptanone. After activation of an aliquot of the organic phase for 1 hour at a flux of 1013 neutrons per cm2, per second, the gamma spectrum is essentially that of tungsten-187. The induced activity is proportional to the concentration of phosphate in the sample. A test of the method showed it to give accurate results at concentrations of 4 to at least 200 p.p.b. of phosphorus when an aliquot of 100 μl. was activated. By suitable reagent purification, counting for longer times, and activation of larger aliquots, the detection limit could be lowered several hundredfold.

  15. Determining endogenous amino acid losses in poultry using single injection of [3H] leucine

    International Nuclear Information System (INIS)

    Three sets of young hens and broilers received six diet treatments. The diets were on fast (FAS), and force-fed nitrogen-free diet (NFD), NFD + 3.20% enzyme hydrolysed casein (EHC), semi-synthesized diets with 5% and 20% crude protein (CP) in which soybean meal was the sole nitrogen source, and semi-synthesized diet with 20% CP in which cotton seed meal was the sole nitrogen source. After force-fed, 30 μCi[3H]Leu/kgBW was injected subcutaneously, the excreta in the following 48h were totally collected, and venous blood samples were taken at 5 min, 30 min, 4 h, 24 h, 36 h and 48 h. The study showed that the ratios between specific radioactivity (SR) of endogenous Leucine in excreta (SRe) and SR of free Leucine in plasma (SRp) kept constant, no matter what kinds of diets the birds ate. This made it possible to determine endogenous amino acid losses (EAAL) of practical diets when NFD was taken as the reference. (authors)

  16. Electrochemical Molecular Imprinted Sensors Based on Electrospun Nanofiber and Determination of Ascorbic Acid.

    Science.gov (United States)

    Zhai, Yunyun; Wang, Dandan; Liu, Haiqing; Zeng, Yanbo; Yin, Zhengzhi; Li, Lei

    2015-01-01

    In this study, electrochemical molecularly imprinted sensors were fabricated and used for the determination of ascorbic acid (AA). Nanofiber membranes of cellulose acetate (CA)/multi-walled carbon nanotubes (MWCNTs)/polyvinylpyrrolidone (PVP) (CA/MWCNTs/PVP) were prepared by electrospinning technique. After being transferred to a glass carbon electrode (GC), the nanofiber interface was further polymerized with pyrrole through electrochemical cyclic voltammetry (CV) technique. Meanwhile, target molecules (such as AA) were embedded into the polypyrrole through the hydrogen bond. The effects of monomer concentration (pyrrole), the number of scan cycles and scan rates of polymerization were optimized. Differential pulse voltammetry (DPV) tests indicated that the oxidation current of AA (the selected target) were higher than that of the structural analogues, which illustrated the selective recognition of AA by molecularly imprinted sensors. Simultaneously, the molecularly imprinted sensors had larger oxidation current of AA than non-imprinted sensors in the processes of rebinding. The electrochemical measurements showed that the molecularly imprinted sensors demonstrated good identification behavior for the detection of AA with a linear range of 10.0 - 1000 μM, a low detection limit down to 3 μM (S/N = 3), and a recovery rate range from 94.0 to 108.8%. Therefore, the electrochemical molecularly imprinted sensors can be used for the recognition and detection of AA without any time-consuming elution. The method presented here demonstrates the great potential for electrospun nanofibers and MWCNTs to construct electrochemical sensors.

  17. Determination of amino acid and protein peroxides by the xylenol orange-Fe(III) complex

    International Nuclear Information System (INIS)

    Oxidative stress imposed on living organisms is believed to lead to the depletion of their antioxidant defences, followed by chemical changes in the cell constituents. These may ultimately develop into pathological conditions such as cancer or cardiovascular disease. An assay of peroxides which could be applied to tissues or simple tissue extracts would prove extremely useful in the studies of the phenomenon of oxidative stress. With this purpose, the authors have tested the ability of two peroxide assay techniques to measure the formation of amino acid and protein peroxides in aqueous solutions irradiated with gamma rays, using a modification of the method based on the oxidation of Fe(II)) by peroxides and complexing of the Fe(III) produced by xylenol orange. The molar extinction coefficients of the peroxides tested were determined by comparison with the well-tested iodometric assay. This work was extended to the detection of all organic peroxides in human blood plasma or serum subjected to oxidative stress, where the iodometric assay proved difficult to apply and unreliable because of the binding of iodine to the blood components. Preliminary results suggest that exposure of serum to gamma radiation leads to immediate peroxidation of the proteins, with a delay before generation of lipid peroxides

  18. Determination of mycophenolic acid in human plasma by ultra performance liquid chromatography tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Vivek Upadhyay; Vikas Trivedi; Gaurang Shah; Manish Yadav; Pranav S. Shrivastav

    2014-01-01

    A simple, sensitive and high throughput ultra performance liquid chromatography tandem mass spectrometry method has been developed for the determination of mycophenolic acid in human plasma. The method involved simple protein precipitation of MPA along with its deuterated analog as an internal standard (IS) from 50 mL of human plasma. The chromatographic analysis was done on Acquity UPLC C18 (100mm*2.1mm,1.7mm) column under isocratic conditions using acetonitrile and 10 mM ammonium formate, pH 3.00 (75:25, v/v) as the mobile phase. A triple quadrupole mass spectrometer operating in the positive ionization mode was used for quantitation. In-source conversion of mycophenolic glucuronide metabolite to the parent drug was selectively controlled by suitable optimization of cone voltage, cone gas flow and desolvation temperature. The method was validated over a wide concentration range of 15–15000 ng/mL. The mean extraction recovery for the analyte and IS was 495%. Matrix effect expressed as matrix factors ranged from 0.97 to 1.02. The method was successfully applied to support a bioequivalence study of 500 mg mycophenolate mofetil tablet in 72 healthy subjects.

  19. Determination of acid ionization constants for weak acids by osmometry and the instrumental analysis self-evaluation feedback approach to student preparation of solutions

    Science.gov (United States)

    Kakolesha, Nyanguila

    One focus of this work was to develop of an alternative method to conductivity for determining the acid ionization constants. Computer-controlled osmometry is one of the emerging analytical tools in industrial research and clinical laboratories. It is slowly finding its way into chemistry laboratories. The instrument's microprocessor control ensures shortened data collection time, repeatability, accuracy, and automatic calibration. The equilibrium constants of acetic acid, chloroacetic acid, bromoacetic acid, cyanoacetic acid, and iodoacetic acid have been measured using osmometry and their values compared with the existing literature values obtained, usually, from conductometric measurements. Ionization constant determined by osmometry for the moderately strong weak acids were in reasonably good agreement with literature values. The results showed that two factors, the ionic strength and the osmotic coefficient, exert opposite effects in solutions of such weak acids. Another focus of the work was analytical chemistry students solution preparation skills. The prevailing teacher-structured experiments leave little room for students' ingenuity in quantitative volumetric analysis. The purpose of this part of the study was to improve students' skills in making solutions using instrument feedback in a constructivist-learning model. After making some solutions by weighing and dissolving solutes or by serial dilution, students used the spectrophotometer and the osmometer to compare their solutions with standard solutions. Students perceived the instrument feedback as a nonthreatening approach to monitoring the development of their skill levels and liked to clarify their understanding through interacting with an instructor-observer. An assessment of the instrument feedback and the constructivist model indicated that students would assume responsibility for their own learning if given the opportunity. This study involved 167 students enrolled in Quantitative Chemical

  20. Meritev izkoristka in nastavitev krmilnih parametrov kaplanove turbine z dolgim cevnim sistemom s primerjalno metodo: Measurement of relative turbine efficiency and adjustment of governing parameters on long penstock Kaplan turbine with comparative method:

    OpenAIRE

    Trebše, Andrej J.

    2004-01-01

    Prispevek obravnava meritev izkoristka kaplanove turbine s primerjalno metodo (test indeks) ter nastavitev delovanja krmilnih sistemov za upravljanje vodilnika in gonilnika. Pri dolgem pretočnem traktu se zaradi večjih izgub vodnega padca med obremenjevanjem stroja spreminja čisti padec. Na podlagi modelnih preizkusov kaplanove turbine in meritve izkoristka turbine na prototipu, smo s primerjalno metodo optimirali krmiljenje vodnega stroja.

  1. Carbon isotopic fractionation in the biosynthesis of bacterial fatty acids. Ozonolysis of unsaturated fatty acids as a means of determining the intramolecular distribution of carbon isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Monson, K.D.; Hayes, J.M. (Indiana Univ., Bloomington (USA). Dept. of Chemistry; Indiana Univ., Bloomington (USA). Dept. of Geology)

    1982-02-01

    Methods for the determination of /sup 13/C abundances at individual olefinic carbon positions have been developed, tested, and shown to perform accurately. (1) The double bond is oxidized with ozone; (2) silver oxide is used to cleave the resulting ozonide quantitatively to carboxylic-acid fragments; (3) a modified Schmidt decarboxylation is used to produce CO/sub 2/ quantitatively from the carboxyl groups of the separated cleavage products; and (4) the CO/sub 2/ is utilized for mass spectrometric analysis. The results of intramolecular isotopic analyses are combined with molecular-average isotopic compositions determined by total combustion in order to show that fatty acids biosynthesized by Escherichia coli grown aerobically with glucose as the sole carbon source and harvested at late log phase are depleted by approximately 3 parts per thousand in /sup 13/C relative to the glucose. This fractionation arises in the formation of acetyl-coenzyme A by pyruvate dehydrogenase and is localized at the carboxyl position in the acetyl-CoA product. The isotopic order in that two-carbon subunit is carried through the biosynthesis of fatty acids so that alternate positions in the fatty-acid chains are depleted in /sup 13/C by an amount equal to twice the molecular-average depletion. The kinetic isotope effect at C-2 for pyruvate dehydrogenase in vivo is shown to be approximately 2.3%.

  2. Carbon isotopic fractionation in the biosynthesis of bacterial fatty acids. Ozonolysis of unsaturated fatty acids as a means of determining the intramolecular distribution of carbon isotopes

    International Nuclear Information System (INIS)

    Methods for the determination of 13C abundances at individual olefinic carbon positions have been developed, tested, and shown to perform accurately. (1) The double bond is oxidized with ozone; (2) silver oxide is used to cleave the resulting ozonide quantitatively to carboxylic-acid fragments; (3) a modified Schmidt decarboxylation is used to produce CO2 quantitatively from the carboxyl groups of the separated cleavage products; and (4) the CO2 is utilized for mass spectrometric analysis. The results of intramolecular isotopic analyses are combined with molecular-average isotopic compositions determined by total combustion in order to show that fatty acids biosynthesized by Escherichia coli grown aerobically with glucose as the sole carbon source and harvested at late log phase are depleted by approximately 3 parts per thousand in 13C relative to the glucose. This fractionation arises in the formation of acetyl-coenzyme A by pyruvate dehydrogenase and is localized at the carboxyl position in the acetyl-CoA product. The isotopic order in that two-carbon subunit is carried through the biosynthesis of fatty acids so that alternate positions in the fatty-acid chains are depleted in 13C by an amount equal to twice the molecular-average depletion. The kinetic isotope effect at C-2 for pyruvate dehydrogenase in vivo is shown to be approximately 2.3%. (author)

  3. Determination of organic acids during the fermentation and cold storage of yogurt.

    Science.gov (United States)

    Fernandez-Garcia, E; McGregor, J U

    1994-10-01

    The objective of the present study was the separation and quantification of orotic, citric, pyruvic, lactic, uric, formic, acetic, propionic, butyric, and hippuric acids in a single isocratic analysis by HPLC. Two methods of extraction were compared: 1) acetonitrile and water and 2) .01N H2SO4. Recoveries of orotic, lactic, acetic, and propionic acids were 90% for both methods. Recoveries of citric, pyruvic, uric, butyric, and hippuric acids were not satisfactory with the acetonitrile method, but were acceptable using the H2SO4 extraction procedure. Yogurts were manufactured under laboratory-scale conditions, and samples were analyzed during fermentation and after storage at 4 degrees C. Samples were analyzed for pH and organic acids. All of the organic acids exhibited varying degrees of increases and decreases during fermentation and storage. Formic and butyric acids were not detected under the conditions of this study.

  4. Determination of Vitamin C and Organic Acid Changes in Strawberry by HPLC During Cold Storage

    Directory of Open Access Journals (Sweden)

    Mehmet Ali KOYUNCU

    2010-12-01

    Full Text Available High pressure liquid chromatographic (HPLC methods were used for measurement of vitamin C and organic acid changes of two strawberry cultivars (‘Dorit’ and ‘Selva’ during cold storage. Harvested strawberries at the last stage of commercial ripeness were placed in perforated (8 perforations, 10 mm diameter plastic boxes and stored at 0°C temperature and 90-95% relative humidity for 10 days. Vitamin C content decreased in both cultivars but no significant differences were found in ‘Dorit’ from the beginning to the end of the storage. The highest share of total acids was contributed by citric acid. It decreased with increase in storage time in both cultivars. Malic acid content of cultivars also decreased with storage time. Tartaric, oxalic and fumaric acid contents fluctuated during storage, but at the end of cold storage these organic acids had decreased in comparison to initial values.

  5. Determination of Ascorbic Acid Using a New Oscillating Chemical System of Lactic Acid-Acetone-BrO3--Mn2+-H2SO4

    Institute of Scientific and Technical Information of China (English)

    YANG,Shu-Tao(杨树涛); LIN,Zhi-Xin(林智信); CAI,Ru-Xiu(蔡汝秀); GAN,Nan-Qin(甘南琴)

    2002-01-01

    Analyte pulse perturbation ( APP ) technique was applied to the study of the perturbation of ascorbic acid (AA) on the lactic acid-acetone-BrO3--Mn2+-H2SO4 oscllating reaction, and AA was determined using this new oscillating chemical system. Influence of experimental variables was investigated. The linear range lies between 5.0 × 10-7-5.5 × 10-5 mol/L, and the precision and throughput were quite good (2.43% as RSD,and 8-10 samples/h, respectively). This method was applied to the determination of real samples and the results were satisfactory. Some aspects of the potential mechanism of action of AA on the oscillating systems are discussed.

  6. 230Th, 232Th and 238U determinations in phosphoric acid fertilizer and process products by ICP-MS

    International Nuclear Information System (INIS)

    Through processing of Santa Quiteria-CE mine phosphate rock, Brazil has established a project for production of phosphoric acid fertilizer and uranium as a by-product. Under leaching conditions of phosphate rock with sulfuric acid, which is the common route for preparing phosphoric acid fertilizer, a large part of uranium, thorium and their decay products naturally present in the rock are solubilized. In order to assess the contamination potential in phosphoric acid and others process products, this paper describes a previous precipitation and direct methods for routine analysis of thorium and uranium isotopes by ICP-MS. In all samples, 230Th, 232Th and 238U were directly determined after dilution, except 230Th in phosphoric acid loaded with uranium sample, which to overcome equipment contamination effect, was determined after its separation by oxalate precipitation using lanthanum as a carrier. The results obtained by the proposed method by ICP-MS, were in good agreement when compared to alpha spectrometry for 230Th, and ICP-OES and spectrophotometry with arsenazo III for elementary uranium and thorium determinations. (author)

  7. Voltammetric determination of polyphenolic content in pomegranate juice using a poly(gallic acid)/multiwalled carbon nanotube modified electrode.

    Science.gov (United States)

    Abdel-Hamid, Refat; Newair, Emad F

    2016-01-01

    A simple and sensitive poly(gallic acid)/multiwalled carbon nanotube modified glassy carbon electrode (PGA/MWCNT/GCE) electrochemical sensor was prepared for direct determination of the total phenolic content (TPC) as gallic acid equivalent. The GCE working electrode was electrochemically modified and characterized using scanning electron microscope (SEM), cyclic voltammetry (CV), chronoamperometry and chronocoulometry. It was found that gallic acid (GA) exhibits a superior electrochemical response on the PGA/MWCNT/GCE sensor in comparison with bare GCE. The results reveal that a PGA/MWCNT/GCE sensor can remarkably enhance the electro-oxidation signal of GA as well as shift the peak potentials towards less positive potential values. The dependence of peak current on accumulation potential, accumulation time and pH were investigated by square-wave voltammetry (SWV) to optimize the experimental conditions for the determination of GA. Using the optimized conditions, the sensor responded linearly to a GA concentration throughout the range of 4.97 × 10(-6) to 3.38 × 10(-5) M with a detection limit of 3.22 × 10(-6) M (S/N = 3). The fabricated sensor shows good selectivity, stability, repeatability and (101%) recovery. The sensor was successfully utilized for the determination of total phenolic content in fresh pomegranate juice without interference of ascorbic acid, fructose, potassium nitrate and barbituric acid. The obtained data were compared with the standard Folin-Ciocalteu spectrophotometric results. PMID:27547628

  8. Study of photorespiration in marine microalgae through the determination of glycolic acid using hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Rigobello-Masini, Marilda; Penteado, José C P; Tiba, Maurício; Masini, Jorge C

    2012-01-01

    Determination of organic acids in intracellular extracts and in the cultivation media of marine microalgae aid investigations about metabolic routes related to assimilation of atmospheric carbon by these organisms, which are known by their role in the carbon dioxide sink. The separation of these acids was investigated by hydrophilic interaction liquid chromatography (HILIC) using isocratic elution with a mobile phase composed of 70:30 v/v acetonitrile/20 mmol/L ammonium acetate buffer (pH 6.8) and detection at 220 nm. HILIC allowed the determinations of glycolic acid, the most important metabolite for the evaluation of the photorespiration process in algae, to be made with better selectivity than that achieved by reversed phase liquid chromatography, but with less detectability. The concentration of glycolic acid was determined in the cultivation media and in intracellular extracts of the algae Tetraselmis gracilis and Phaeodactylum tricornutum submitted to different conditions of aeration: (i) without forced aeration, (ii) aeration with atmospheric air, and (iii) bubbling with N(2). The concentration of glycolic acid had a higher increase as the cultures were aerated with nitrogen, showing higher photorespiratory flux than that occurring in the cultures aerated with atmospheric air.

  9. Determination of haloacetic acids concentrations in hospital effluent after chlorination by ion chromatography

    Institute of Scientific and Technical Information of China (English)

    SUN Ying-xue; GU Ping

    2007-01-01

    The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids(HAAs),a calss of disinfection by-products formed as a result of chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples' turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and were found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L respectively, and the other three are ranging from 0.48 to 0.82 μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid is the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.

  10. Determination of amino acids in Chinese rice wine by fourier transform near-infrared spectroscopy.

    Science.gov (United States)

    Shen, Fei; Niu, Xiaoying; Yang, Danting; Ying, Yibin; Li, Bobin; Zhu, Geqing; Wu, Jian

    2010-09-01

    Chinese rice wine is abundant in amino acids. The possibility of quantitative detection of 16 free amino acids (aspartic acid, threonine, serine, glutamic acid, proline, glycine, alanine, valine, methionine, isoleucine, leucine, tyrosine, phenylalanine, lysine, histidine, and arginine) in Chinese rice wine by Fourier transform near-infrared (NIR) spectroscopy was investigated for the first time in this study. A total of 98 samples from vintage 2007 rice wines with different aging times were analyzed by NIR spectroscopy in transmission mode. Calibration models were developed using partial least-squares regression (PLSR) with high-performance liquid chromatography (HPLC) by postcolumn derivatization and diode array detection as a reference method. To validate the calibration models, full cross (leave-one-out) validation was employed. The results showed that the calibration statistics were good (rcal>0.94) for all amino acids except proline, histidine, and arginine. The correlation coefficient in cross validation (rcv) was >0.81 for 12 amino acids. The residual predictive deviation (RPD) value obtained was >1.5 in all amino acids except proline and arginine, and it was >2.0 in 6 amino acids. The results obtained in this study indicated that NIR spectroscopy could be used as an easy, rapid, and novel tool to quantitatively predict free amino acids in Chinese rice wine without sophisticated methods. PMID:20707307

  11. Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02 × 10−7–5.23 × 10−4 mol L−1 and 1.43 × 10−7–4.64 × 10−4 mol L−1, the detection limits were 1.12 × 10−8 mol L−1 and 2.24 × 10−8 mol L−1, respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. - Graphical abstract: The schematic diagram of formation of Au nanotube arrays (a) and the stepwise procedure of the sensor (b). Highlights: ► Gold nanotubes array has been synthesized by cyclic voltammetry. ► The mechanism of deposition of gold nanotube has been discussed. ► A determination of ascorbic acid and uric acid was constructed by gold array. ► A satisfied determination of samples can be obtained by this sensor.

  12. Simultaneous determination of amino acids and carbohydrates in culture media of Clostridium thermocellum by valve-switching ion chromatography.

    Science.gov (United States)

    Fa, Yun; Yang, Haiyan; Ji, Chengshuai; Cui, He; Zhu, Xinshu; Du, Juan; Gao, Jun

    2013-10-10

    An improved method for the simultaneous determination of 20 amino acids and 7 carbohydrates using one-valve switching after injection, ion chromatography, and integrated pulsed amperometric detection is proposed. The resolution of the amino acids and carbohydrates in the cation trap column was investigated. In addition, parameters including flow liquid type, flow rate, concentration, and valve-switch timing were optimized. The method is time-saving, effective, and accurate for the simultaneous separation of amino acids and carbohydrates, with a mean correlation coefficient of >0.99 and repeatability of 0.5-4.6% for eight replicates. The method was successfully applied in the analysis of amino acids and carbohydrates in aseptic media and in extracellular culture media of three phenotypes of Clostridium thermocellum.

  13. Kinetic Determination of Uric Acid in Human Serum by Using the Uncatalyzed BZ Reaction in Non-equilibrium Steady State

    Institute of Scientific and Technical Information of China (English)

    Ren, Jie; Yang, Wu; Niu, Xiuli; Gao, Jinzhang

    2012-01-01

    A novel kinetic method for determination of uric acid in human serum by means of an uncatalyzed BZ system consisting of potassium bromate and p-hydroxybenzaldehyde (p-HBA) in sulfuric acid medium was proposed, in which the analyte perturbation to the system was recorded close to the bifurcation point. The potential change was directly proportional to the logarithm of concentration of uric acid in the range of 3.73 × 10 8--7.48 × 10-4 mol.L-1 (r=0.9983) with a detection limit of 7.45 × 10-9mol.L-I and a recovery from 98.9% to 101.1%. A comparison between the proposed technique and other methods indicated that results obtained were in agreement with those in clinical detection. In addition, the possible mechanism of action of uric acid on the uncatalyzed BZ reaction was also discussed briefly.

  14. Protein quality as determined by the Digestible Indispensable Amino Acid Score: evaluation of factors underlying the calculation.

    Science.gov (United States)

    Wolfe, Robert R; Rutherfurd, Shane M; Kim, Il-Young; Moughan, Paul J

    2016-09-01

    The Food and Agriculture Organization of the United Nations recently recommended the adoption of a new and improved scoring system (Digestible Indispensable Amino Acid Score [DIAAS]) to quantify dietary protein quality. The DIAAS is based on the relative digestible content of the indispensable amino acids (IAAs) and the amino acid requirement pattern. Factors involved in calculation of the DIAAS include: use of the content and profile of IAAs as the basis for quality; methods for determination of the protein and amino acid content of the protein source; accuracy of individual requirement values for IAAs; normalization of IAA requirements by the estimated average requirement for protein; and basing the DIAAS on the true ileal digestibility of each IAA in the test protein. This review outlines the rationale for including each of these factors in the calculation of the DIAAS and describes associated potential errors. PMID:27452871

  15. Determination of the 13C contents of organic acids and sugars in fruit juices: an inter-comparison study

    International Nuclear Information System (INIS)

    The determination of the repeatability (r) and reproducibility (R) of the (13C/12C) measurement in sugars and organic acids contained in different fruit juices was conducted on an international basis involving 17 laboratories. The mean values of rper thousand (Rper thousand) for acids and sugars are, respectively, equal to 0.58 (1.75) and 0.34 (0.71) and the relatively large values observed for R of acid determinations are related to the preparation step. However, the least significant difference computed for several pairs of natural and spiked juices indicate that the 13C method can be applied for detecting fruit juice adulteration. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  16. Determination of the {sup 13}C contents of organic acids and sugars in fruit juices: an inter-comparison study

    Energy Technology Data Exchange (ETDEWEB)

    Guillou, C. [JCR-ISPRA, Environment Institute, Food and Drug Analysis and Consumer Protection Unit, TP740, via Fermi 2, 21020 Ispra (Italy); Koziet, J. [Pernod Ricard, 120, av du Marechal Foch, 94015 Creteil cedex (France); Rossmann, A. [Lehrstuhl fuer Allgemeine Chemie und Biochemie, TUM, D-85350 Freising-Weihenstephan (Germany); Martin, G.J. [CEAIS, Site de la Geraudiere, Rue PA Bobierre, BP 72304, 44323 3 Nantes cedex (France)

    1999-05-03

    The determination of the repeatability (r) and reproducibility (R) of the ({sup 13}C/{sup 12}C) measurement in sugars and organic acids contained in different fruit juices was conducted on an international basis involving 17 laboratories. The mean values of rper thousand (Rper thousand) for acids and sugars are, respectively, equal to 0.58 (1.75) and 0.34 (0.71) and the relatively large values observed for R of acid determinations are related to the preparation step. However, the least significant difference computed for several pairs of natural and spiked juices indicate that the {sup 13}C method can be applied for detecting fruit juice adulteration. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  17. A novel method for the determination of ascorbic acid and antioxidant capacity in Opuntia ficus indica using in vivo microdialysis.

    Science.gov (United States)

    Pretti, L; Bazzu, G; Serra, P A; Nieddu, G

    2014-03-15

    A simple and rapid method was developed for in vivo simultaneous determination of ascorbic-acid and antioxidant capacity in microdialysates from cladodes of Opuntia ficus-indica (L.) Miller. The method is verified in water-stressed plants, as compared with a well-watered test controls. The microdialysis probe construction and insertion procedure was specifically developed to minimise the tissue trauma of the plant and to obtain optimal dialysis performance. Microdialysis was performed using a flow rate of 3 μL/min and the samples were analysed by HPLC coupled to electrochemical detection of ascorbic-acid and DPPH-determined antioxidant capacity. Our data indicate exponential decay of the concentrations of the analysed compounds as a function of microdialysis sampling time. Water-stressed Opuntia show decreased ascorbic acid levels and increased the others antioxidants. PMID:24206696

  18. A novel method for the determination of ascorbic acid and antioxidant capacity in Opuntia ficus indica using in vivo microdialysis.

    Science.gov (United States)

    Pretti, L; Bazzu, G; Serra, P A; Nieddu, G

    2014-03-15

    A simple and rapid method was developed for in vivo simultaneous determination of ascorbic-acid and antioxidant capacity in microdialysates from cladodes of Opuntia ficus-indica (L.) Miller. The method is verified in water-stressed plants, as compared with a well-watered test controls. The microdialysis probe construction and insertion procedure was specifically developed to minimise the tissue trauma of the plant and to obtain optimal dialysis performance. Microdialysis was performed using a flow rate of 3 μL/min and the samples were analysed by HPLC coupled to electrochemical detection of ascorbic-acid and DPPH-determined antioxidant capacity. Our data indicate exponential decay of the concentrations of the analysed compounds as a function of microdialysis sampling time. Water-stressed Opuntia show decreased ascorbic acid levels and increased the others antioxidants.

  19. Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase)

    International Nuclear Information System (INIS)

    A study on the optimization and development of a chromatographic method for the determination of gallic and picric acids in pyrotechnic samples is presented. In order to achieve this, both analytical conditions by HPLC with diode detection and extraction step of a selected sample were studied. (Author)

  20. A Comprehensive Evaluation of the Melting Points of Fatty Acids and Esters Determined by Differential Scanning Calorimetry

    Science.gov (United States)

    The melting point is one of the most important physical properties of a chemical compound and plays a significant role in determining possible applications. For fatty acid esters the melting point is essential for a variety of food and non-food applications, the latter including biodiesel and its c...

  1. Determination of urinary 18 beta-glycyrrhetinic acid by gas chromatography and its clinical application in man

    NARCIS (Netherlands)

    Guillaume, CPF; van der Molen, JC; Kerstens, MN; Dullaart, RPF; Wolthers, BG

    1999-01-01

    A sensitive and quantitative gas chromatographic assay for the determination of 18 beta-glycyrrhetinic acid (18 beta-GA), the main metabolite of glycyrrhizin after oral licorice consumption in human urine, has been developed and validated. For the extraction of 18 beta-GA from urine two Sep-Pak C-18

  2. Determining a Robust D-Optimal Design for Testing for Departure from Additivity in a Mixture of Four Perfluoroalkyl Acids.

    Science.gov (United States)

    Our objective is to determine an optimal experimental design for a mixture of perfluoroalkyl acids (PFAAs) that is robust to the assumption of additivity. PFAAs are widely used in consumer products and industrial applications. The presence and persistence of PFAAs, especially in ...

  3. Impedimetric test for rapid determination of performic acid (PFA biocidal activity toward Echerichia coli

    Directory of Open Access Journals (Sweden)

    Małgorzata Lasik

    2013-12-01

    Full Text Available   Background. Performic acid has recently become available on a commercial scale for potential use in waste-water disinfection and can become an innovative biocide for various purposes in food processing. The aim of our study was: 1 to investigate the antimicrobial resistance of performic acid as high active and non toxic chemical disinfectant against Escherichi coli (hygiene indicator test  microorganism used in industrial micro- biology and 2 to evaluate the electrical impedance measurement method usefulness for fast and high precise test of antibacterial activity. Material and methods. Four types of antimicrobial disinfectants (commercial 35% hydrogen peroxide, 1% performic acid, 35% hydrogen peroxide and 15% formic acid were tested against Escherichia coli as hygiene indicator test microorganism. By evaluating the biocidal activity of selected disinfectants two methods were compared: electrical impedance measurement and classical serial dilution method with turbidity effect. Results.  It was stated that the performic acid expressed the highest antibacterial activity in comparison to other tested peroxide disinfectants: commercial 35% hydrogen peroxide solution and components required for performic acid production: 35% hydrogen peroxide solution with stabilizers and 15% formic acid solution with stabilizers. It was demonstrated that the proposed alternative microbiology method of electrical imped- ance measurement facilitates a rapidly and more precise analyses of the intensity of disinfectants inhibition effect. Conclusions. It can be postulated that both, the performic acid disinfectants as well as the impedimetric method can be a good advantage in the industrial microbiology.  

  4. [Determination of the nucleic acids in pig embryonic kidney cells by magnetic cytaphoresis].

    Science.gov (United States)

    Chikov, V M; Maksimova, E V

    1989-01-01

    Gallocyanine-chrome alum-stained pig embryonic kidney cells have paramagnetic properties. They move under the influence of gradient magnetic field (magnetophoresis). The velocity of magnetophoresis is proportional to the content of nucleic acids in cells. This allows to estimate the content of nucleic acids per cell dry weight by magnetophoresis and analytical centrifugation. PMID:2473104

  5. Preparation of sphingolipid fatty acid methyl esters for determination by gas-liquid chromatography.

    Science.gov (United States)

    MacGee, J; Williams, M G

    1981-01-30

    Sphingolipid fatty acids are first converted to a mixture of free acids and their n-butyl esters by heating the specimen at 85 degree C in aqueous butanolic hydrogen chloride; the butyl esters are then saponified with methanolic potassium hydroxide. After acidification and extraction into hexane, the fatty acids are extracted into a very small volume of aqueous trimethyl(m-trifluorotolyl)ammonium hydroxide (TMTFTH), injection of an aliquot of the TMTFTH extract into the gas chromatograph yields the fatty acid methyl esters by pyrolytic methylation of the quaternary ammonium salts of the fatty acids. The preparation of a specimen ready for the gas--liquid chromatographic (GLC) analysis with quantitative recovery of the sphingolipid fatty acids can be accomplished in less than 2 h. By comparison, none of a number of well-accepted techniques for the release of sphingomyelin fatty acids by hydrolysis or methanolysis released the fatty acids quantitatively in less than 3 h, and all required additional manipulations before GLC analysis. PMID:7217267

  6. New insight into the SSC8 genetic determination of fatty acid composition in pigs

    NARCIS (Netherlands)

    Revilla, M.; Ramayo-Caldas, Y.; Castello, A.; Corominas, J.; Puig-Oliveras, A.; Ibanez-Escriche, N.; Munoz, M.; Ballester, M.; Folch, J.M.

    2014-01-01

    BACKGROUND: Fat content and fatty acid composition in swine are becoming increasingly studied because of their effect on sensory and nutritional quality of meat. A QTL (quantitative trait locus) for fatty acid composition in backfat was previously detected on porcine chromosome 8 (SSC8) in an Iberia

  7. Experimental evaluation of fatty acid profiles as a technique to determine dietary composition in benthic elasmobranchs.

    Science.gov (United States)

    Beckmann, Crystal L; Mitchell, James G; Seuront, Laurent; Stone, David A J; Huveneers, Charlie

    2013-01-01

    Fatty acid (FA) analysis is a tool for dietary investigation that complements traditional stomach content analyses. Controlled feeding experiments were used to determine the extent to which the FA composition of diet is reflected in the liver and muscle tissue of the Port Jackson shark Heterodontus portusjacksoni. Over 10 wk, two groups of sharks were fed prawns or squid, which have distinct FA profiles. The percentage of total FA was significantly different for shark liver and muscle tissue when comparing controls with prawn- and squid-fed sharks. Compared with experimentally fed sharks, control shark muscle and liver had higher levels of 18:1n-9 and 20:2n-9. When comparing prawn- and squid-fed sharks, only liver tissue showed a significant difference in FA profiles. The livers of prawn-fed sharks were comparatively higher in 18:1n-7, 22:5n-3, 20:0, and 18:1n-9, while the squid-fed sharks had higher levels of 16:0 and 22:6n-3. These FAs in shark liver tissue were all reflective of higher amounts in their respective dietary items, demonstrating the conservative transfer of FA from diet to liver tissue. This study shows that liver and muscle FA profiles can be used as indicators of dietary change through the comparison of controls and fed sharks. The timescale of this study may not have been sufficient for capturing the integration of FA into muscle tissue because only liver FA profiles were useful to distinguish between sharks fed different diets. These findings have important implications for sampling design where FA profiles are used to infer dietary preferences. PMID:23434786

  8. Molecular Determinants of the Response of Tumor Cells to Boswellic Acids

    Directory of Open Access Journals (Sweden)

    Thomas Efferth

    2011-08-01

    Full Text Available Frankincense (Boswellia serrata, B. carterii is used as traditional remedy to treat inflammatory diseases. The molecular effects of the active ingredients, the boswellic acids, on the immune system have previously been studied and verified in several clinical studies. Boswellic acids also inhibit cancer cell growth in vitro and in vivo. The molecular basis of the cytotoxicity of boswellic acids is, however, not fully understood as yet. By mRNA-based microarray, COMPARE, and hierarchical cluster analyses, we identified a panel of genes from diverse functional groups, which were significantly associated with sensitivity or resistance of a- or b-boswellic acids, such as transcription factors, signal transducers, growth regulating genes, genes involved in RNA and protein metabolism and others. This indicates that boswellic acids exert profound cytotoxicity on cancer cells by a multiplicity of molecular mechanisms.

  9. 饲用酸化剂中甲酸、乙酸、丙酸、乳酸、柠檬酸的同步测定%Determination of formic acid, acetic acid, propionic acid, lactic acid, citric acid in feed acidifier

    Institute of Scientific and Technical Information of China (English)

    索德成; 李兰; 樊霞

    2012-01-01

    A method of the simultaneous determination of the contents of formic acid, acetic acid, propionic acid, lactic acid, citric acid in feed acidifier by HPLC was established. The separation was performed on Grom-Silorg acid(250 mm×4.6 mm, 5 μm) with the mobile phase of hydrochloric acid solution (pH 2.5)/The detection wave length was 210 nm.The flow rate was 1,0 ml/min and the column temperature was 30 ℃.Good linearities of five acid were showed. The average recoveries were greater than 85% respectively, RSD was less than 10.0%.The result of real sample have been shown: the method was simple, rapid and reliable for the simultaneous determination of formic acid, acetic acid, propionic acid, lactic acid, citric acid in organic acids.%实验建立利用高效液相色谱同时测定饲用酸化剂中甲酸、乙酸、丙酸、乳酸、柠檬酸含量的方法.采用Grom-Sil org acid柱(250 mm×2.1 mm,5μm)进行分析.流动相为pH值2.5磷酸水溶液;流速为1.0 ml/min;检测波长为210 nm;柱温为30℃.在此色谱条件下,5种有机酸分离良好.平均回收率均大于85%,RSD小于10.0%.对实际样品的检测结果表明:该方法操作简便易行,准确可靠.

  10. Determination of 5-caffeoylquinic acid (5-CQA as one of the major classes of chlorogenic acid in commercial tea and coffee samples

    Directory of Open Access Journals (Sweden)

    Grujić-Letić Nevena

    2015-01-01

    Full Text Available Background/Aim. Tea and coffee are one of the most widely consumed beverages in the world due to their beneficial health effects which are largely associated with their phenolic compounds composition, including chlorogenic acid. The main aim of this study was to determine 5-caffeoylquinic acid (5-CQA, as one of the major classes of chlorogenic acid, in various commercial tea and coffee samples present at the Serbian market. Methods. A high-performance liquid chromatography (HPLC method for determination of 5-CQA in plant extracts was applied to determine the content of this active compound in commercial tea and coffee samples. Mobile phase was aqueous 1.5% acetic acid - methanol (80:20, v/v with the flow rate of 0.8 mL/min. Run time was 15 min and column temperature 25°C. The detection was performed at 240 nm. Results. The HPLC method was modified and revalidated. The 5-CQA content varied depending on the type of tea (white, green, black tea and mate and the processing technology. Green tea had the highest 5-CQA content (16 mg/100 mL among the analyzed tea samples. The content of 5-CQA in coffee samples ranged 0-36.20 mg/g of coffee and 0-46.98 mg/100 mL of beverage, showing that the content varied depending on the type of coffee, coffee processing technology and the formulation. Conclusion. The modified and revalidated HPLC method showed a good accuracy, repeatability, selectivity and robustness. The highest amount of 5-CQA was determined in green tea in comparison to white, black and mate tea because the increased oxidation level decreases the amount of 5-CQA. The obtained results for commercial coffee samples indicated that the formulation was the most important factor determining the amount of 5-CQA. It can be concluded that plant material selection, processing conditions and formulation have great influence on the amount of chlorogenic acid (5-CQA in the final tea and coffee products. [Projekat Ministarstva nauke Republike Srbije, br. OI

  11. Solubilization of amphiphilic carboxylic acids in nonionic micelles: determination of partition coefficients from pKa measurements and NMR experiments.

    Science.gov (United States)

    Dupont-Leclercq, Laurence; Giroux, Sébastien; Henry, Bernard; Rubini, Patrice

    2007-10-01

    The solubilization of octylamidotartaric acid (C8T) and octanoic acid (C8C) in Triton X-100 and Brij 58 nonionic micelles has been studied by pHmetric and 1H NMR self-diffusion experiments. As both C8C and C8T exhibit acid-base properties, a distinction between the partition of the neutral acidic form, in terms of the partition coefficient KPH, and the partition of the charged basic form, in terms of the partition coefficient KP-, has been made. The acidity constants, Ka, of C8T and C8C in the presence of micelles have been evaluated from pHmetric experiments. For both solutes, an increase in the pKa is observed in micellar media due to the difference in the partition of acidic and basic forms of the solutes. A model has been developed to determine KPH and KP- from the pKa shifts observed. The values obtained by this pKa shift modeling method and those from self-diffusion coefficient measurements are in good agreement. The acidic form of C8C is incorporated to a larger extent into the Brij 58 micelles than the acidic form of C8T, whereas the opposite trend is observed for the basic forms. Both the acidic and basic forms of C8T are more easily incorporated into Brij 58 micelles than into Triton X-100 micelles. The influence of the structure of the polar head on the solubilization properties is demonstrated. Moreover, evidence for the localization of the solutes in the micelles is obtained from the comparison of the partition coefficients and from 1H NMR data. PMID:17850105

  12. Comparison of acid ethanol extraction and acid gel filtration prior to IGF-I and IGF-II radioimmunoassays; Improvement of determinations in acid ethanol extracts by the use of truncated IGF-I as radioligand

    Energy Technology Data Exchange (ETDEWEB)

    Bang, P.; Eriksson, U.; Wivall, I.-L.; Hall, K. (Department of Endocrinology, Karolinska Institute, Stockholm (Sweden)); Sara, V. (Department of Pathology, Karolinska Institute, Stockholm (Sweden))

    1991-01-01

    Insulin-like growth factor binding proteins interfere in the IGF-I and -II radioimmunoassays. In an attempt to overcome this problem, we have compared the use of truncated IGF-I, with reduced IGFBP affinity, and IGF-I as radioligands for IGF-I RIA measurements in serum separated by acid gel filtration or acid ethanol extraction followed by cryo-precipitation. With truncated IGF-I as radioligand the IGF-I measurements in acid gel filtrates and acid ethanol extracts were significantly correlated in healthy subjects (N=42, r=0.91, p<0.001) and in patients with acromegaly (N=10, r=0.85, p<0.01), GH deficiency (N=10, r=0.88, p<0.001) or Type I diabetes mellitus (N=10, r=0.90, p<0.001). In contrast, the IGF-I concentrations in acid ethanol extracts determined with IGF-I as radioligand did not correlate with those in acid gel filtrates using truncated IGF-I radioligand in patients with acromegaly (r=0.61, NS) or GH deficiency (r=0.46, NS). In the latter group the mean IGF-I concentrations measured in acid ethanol extracts were erroneously elevated by 112%. Low-affinity antibodies used for IGF-II RIA determinations failed to give reliable results in acid ethanol extracts from patients with Type I diabetes mellitus or GH deficiency. In conclusion, erroneously high IGF-I concentrations owing to binding of the radioligand to IGFBPs not completely removed by acid ethanol extraction can be avoided by the use of truncated IGF-I as radioligand. (author).

  13. Determination of naphthenic acid profile in Ghana's Jubilee Oil using gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Crude oil is the life-blood of the global economy. Its importance stems from the fact that it is a base product for a wide variety of goods [Drugs, Plastics, Liquefied Petroleum Gas (LPG)]. The oil discovery (over 3 billion barrel reserves in hydrocarbon and gas), about 60 km offshore between the Deepwater Tano and Cape Three Points Block in South western Ghana is a valuable natural asset and it has the potential of boosting the Ghanaian economy. During petroleum processing, various waste products are generated. One of such products is Naphthenic acids (NA). Naphthenic acids are organic acids naturally occurring in crude oil and a constituent of waste associated with oil refinery. Naphthenic acids serve as biomarkers for identification of the source of crude oil. The presence of Naphthenic acid in the aquatic environment causes toxic effects due to their weak biodegradable nature; the toxicity of Naphthenic acids depends on the class of Naphthenic acids present in the crude oil. The study assessed the profile of Naphthenic acids in Ghana’s Jubilee crude oil using Low Resolution Electron Impact – Gas Chromatography Mass Spectrometry (LREI-GCMS) after isolation of Naphthenic acids in the Jubilee oil by a modified Kupchan’s Partitioning Process. The Mass Spectrometric (MS) Work Station Software was used for the identification of the Naphthenic acids present in the Jubilee crude oil. The quality of the Jubilee oil was also evaluated through the use of some key physico-chemical parameters [Total Acid Number (TAN), Sulphur Content, Viscosity, Pour Point, Flashpoint, Water Content and Densities] based on the American Standards for Testing and Materials (ASTM, 2007). The Total Acid Number was determined by Colorimetric Titration (ASTM D974); Sulphur Content by X-ray Fluorescent Spectrometry (ASTM D4294); Pour Point by the use of the SETA cloud and Pour Point Refrigerator Technique (ASTM D97); Viscosity by Gravity Timed Method (ASTM D445); Density by the Hydrometer

  14. Quantitative determination of uric acid using CdTe nanoparticles as fluorescence probes.

    Science.gov (United States)

    Jin, Dongri; Seo, Min-Ho; Huy, Bui The; Pham, Quoc-Thai; Conte, Maxwell L; Thangadurai, Daniel; Lee, Yong-Ill

    2016-03-15

    A convenient enzymatic optical method for uric acid detection was developed based on the fluorescence quenching of ligand-capped CdTe nanoparticles by H2O2 which was generated from the enzymatic reaction of uric acid. The interactions between the CdTe nanoparticles capped with different ligands (glutathione, 3-mercaptopropionic acid, and thioglycerol) and H2O2 were investigated. The fluorescence quenching studies of GSH-capped CdTe nanoparticles demonstrated an excellent sensitivity to H2O2. The effects of uric acid, uricase and H2O2 on the fluorescence intensity of CdTe nanoparticles were also explored. The detection conditions, reaction time, pH value, incubation period and the concentration of uricase and uric acid were optimized. The detection limit of uric acid was found to be 0.10 µM and the linear range was 0.22-6 µM under the optimized experimental conditions. These results typify that CdTe nanoparticles could be used as a fluorescent probe for uric acid detection. PMID:26433069

  15. Determination and stereochemistry of proteinogenic and non-proteinogenic amino acids in Saudi Arabian date fruits.

    Science.gov (United States)

    Ali, Hatem Salama Mohamed; Alhaj, Omar Amin; Al-Khalifa, Abdulrahman Saleh; Brückner, Hans

    2014-09-01

    Whereas an abundance of literature is available on the occurrence of common proteinogenic amino acids (AAs) in edible fruits of the date palm (Phoenix dactylifera L.), recent reports on non-proteinogenic (non-coded) AAs and amino components are scarce. With emphasis on these components we have analyzed total hydrolysates of twelve cultivars of date fruits using automated ion-exchange chromatography, HPLC employing a fluorescent aminoquinolyl label, and GC-MS of total hydrolysates using the chiral stationary phases Chirasil(®)-L-Val and Lipodex(®) E. Besides common proteinogenic AAs, relatively large amounts of the following non-proteinogenic amino acids were detected: (2S,5R)-5-hydroxypipecolic acid (1.4-4.0 g/kg dry matter, DM), 1-aminocyclopropane-1-carboxylic acid (1.3-2.6 g/kg DM), γ-amino-n-butyric acid (0.5-1.2 g/kg DM), (2S,4R)-4-hydroxyproline (130-230 mg/kg DM), L-pipecolic acid (40-140 mg/kg DM), and 2-aminoethanol (40-160 mg/kg DM) as well as low or trace amounts (amino acids in date fruits is briefly addressed.

  16. [Simultaneous determination of 16 organic acids in feed additives by on-line enrichment and ion chromatography-mass spectrometry].

    Science.gov (United States)

    Xiong, Zhiyu; Dong, Ying; Zhou, Hongbin; Yu, Yang; Li, Jing; Sun, Li

    2014-02-01

    A novel analytical method for simultaneous determination of sixteen organic acids by on-line enrichment and ion chromatography-mass spectrometry (IC-MS) was developed. Online enrichment and separation of the organic acids were performed by ion chromatography on a homemade enrichment column and a homemade separation column. The qualitative and quantitative analyses of the organic acids were performed by mass spectrometry in selected ion monitoring (SIM) mode on the basis of atmospheric pressure chemical ionization (APCI) source in negative mode. The sample of 200 microL was injected for the analysis, and the on-line enrichment time was 3 min. The sodium hydroxide solution was used as a gradient elution system. The two columns made it possible to have a low limit of detection due to the good enrichment and separation capability. The sixteen organic acids were separated completely within 30 min. All curves showed good linearity within the test concentration ranges. The limits of detection (LODs) were between 0.01 and 0.22 mg/L, and the average recoveries were between 70.6% and 110.8%. The relative standard deviations (RSDs) were less than 6.3%. The results indicate that this method is simple, rapid, sensitive and accurate for the determination of the organic acids in feed additives.

  17. Simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture by high performance liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    Zhi-Sheng Xie; Xin-Jun Xu; Chun-Yan Xie; Jie-Yun Huang; Mei Yang; Rui-Ming Li; Xiao Chen

    2011-01-01

    A reversed phase high performance liquid chromatography (HPLC) method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 column (250 mm × 4.6 mm, 5 μm) was used as the stationary phase and the mobile phase was composed of acetonitrile and aqueous phosphoric acid (0.2%, v/v). Gradient elution was carried out at the flow rate of 1.0 mL/min and the column temperature was 30 ℃. An ultraviolet (UV) detector was used with a selected wavelength of 240 nm. Calibration curves were linear within the concentration range of 4.6-45.75 μg/mL for 12, 13-dihydroxyeuparin (r〉0.9999) and 106.9-1068.9μg/mL for glycyrrhizic acid (r〉0.9999), respectively. Recoveries were 102.18% for 12, 13-dihydroxyeuparin and 101.17% for glycyrrhizic acid. The method developed could be applied to the simultaneous determination of 12, 13- dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture.

  18. 灵芝中灵芝酸的测定研究%Determination of Ganoderma Lucidum Acid by HPLC

    Institute of Scientific and Technical Information of China (English)

    孙金旭

    2015-01-01

    The HPLC determination method for the determination of Ganoderma lucidum acid was established. The result showed that the maximum standard deviation of cholesterol content was 1.36%under this method for determination and Cholesterol content displayed an excellent linear relationship , the standard curve equation was Y=625.71x+82.857(R=0.998 2). The spike recoveries for cholesterol were between 97.04%and 102.64%, the method was feasibility and accurate for using to determine Ganoderma lucidum acid, the average contents of Ganoderma lucidum acid was 1.03 mg/g by HPLC determination.%利用HPLC法测定灵芝中灵芝酸含量的方法,此方法测定灵芝中灵芝酸含量重复性试验最大标准偏差为1.36%,峰面积与灵芝酸标品线性关系良好,标准曲线方程为Y=625.71x+82.857(R=0.9982),加标回收率在97.04%~102.64%之间,此方法用于灵芝中灵芝酸含量准确、可行;经测定灵芝中灵芝酸为含量1.03 mg/g。

  19. Ascorbic Acid Determination in Commercial Fruit Juice Samples by Cyclic Voltammetry

    OpenAIRE

    Slawomir Kalinowski; Aurelia Magdalena Pisoschi; Andrei Florin Danet

    2008-01-01

    A method was developed for assessing ascorbic acid concentration in commercial fruit juice by cyclic voltammetry. The anodic oxidation peak for ascorbic acid occurs at about 490 mV on a Pt disc working electrode (versus SCE). The influence of the potential sweep speed on the peak height was studied. The obtained calibration graph shows a linear dependence between peak height and ascorbic acid concentration in the domain (0.1–10 mmol·L−1). The equation of the calibration graph was y = 6.391x +...

  20. pfaB products determine the molecular species produced in bacterial polyunsaturated fatty acid biosynthesis

    OpenAIRE

    Orikasa, Yoshitake; TANAKA, Mika; Sugihara, Shinji; Hori, Ryuji; Nishida, Takanori; Ueno, Akio; Morita, Naoki; Yano, Yutaka; Yamamoto, Kouhei; SHIBAHARA, Akira; Hayashi, Hidenori; Yamada, Yohko; Yamada, Akiko; Yu, Reiko; Watanabe, Kazuo

    2009-01-01

    When pDHA4, a vector carrying all five pfaA-pfaE genes responsible for docosahexaenoic acid (DHA; 22:6) biosynthesis in Moritella marina MP-1, was coexpressed in Escherichia coli with the individual pfaA-pfaD genes for eicosapentaenoic acid (EPA; 20:5) biosynthesis from Shewanella pneumatophori SCRC-2738, both polyunsaturated fatty acids were synthesized only in the recombinant carrying pfaB for EPA synthesis. Escherichia coli coexpressing a deleted construct comprising pfaA, pfaC, pfaD and p...

  1. EFFECT OF SURFACTANT SDS ON DETERMINATION OF NUCLEIC ACID WITH TERBIUM (III)FLUO

    Institute of Scientific and Technical Information of China (English)

    WuHui; WanYu

    2002-01-01

    The effect of an anionic surfactant(sodium dodecylsulfate.SDS)on the fluorescence properties of nucleic acid with terbium(III)is studied.Results show that ri-bonucleir acid (RNA)presents fluorescence reaction with Tb(III)directly.but deoxyribonucleic acid(DNA)pre-sents similar fluorescence reaction only after its denatura-tion.In the presence of SDS ,the fluorescence intensity is 4.0 times and 3.5 times greater than that of DNA and RNA without SDS.

  2. Gas chromatography determination of fatty acid alkyl esters (methyl and ethyl in the presence of mono., di- and triglycerides

    Directory of Open Access Journals (Sweden)

    Paulo César Narváez Rincón

    2010-04-01

    Full Text Available Determining fatty acid methyl or ethyl esters, in the presence of mono-, di- and tri glycerides, is very important when studying fatty compounds' methanolysis or ethanolysis, as well as for controlling the quality of petrochemical products. This work presents a useful technique for determining fatty acids methyl or ethyl esters by high temperature gas chromastography in the presence of mono-, di- and triglycerides. Samples were silylated with N, O-bis (trimethylsilyl trifluroacetamide (BSTFA and then passed throught a 12m HT5 column coated with a phenyl-polysiloxane-carborane film. Standard methyl and ethyl palmitate, methyl and ethyl oleate, DL-palmitin, dipalmitin, tripalmitin and triolein solutions were used for calibrating the technique, using tricaprin as internal standard. Retention times and response factors were also determined. The results were employed in following-up palm oil methanolysis and ethanolysis reactions.

  3. Determination of the acid values of edible oils via FTIR spectroscopy based on the OH stretching band.

    Science.gov (United States)

    Jiang, Xiuming; Li, Shen; Xiang, Guoqiang; Li, Qiuhong; Fan, Lu; He, Lijun; Gu, Keren

    2016-12-01

    A new method for determining the acid values (AVs) of edible oils based on the OH stretching band was developed. The oil sample was diluted with carbon tetrachloride and was placed in a quartz cuvette with a thickness of 1cm to record the FTIR spectrum. The peak at 3535cm(-1), which corresponds to the OH stretch of the carboxyl group in free fatty acids, together with the peak valley at 3508cm(-1) and the spectral data in the range of 3340-3390cm(-1) were used to determine the AV of the edible oil. The excellent linear relationship between the AVs measured in this work and those measured using a titration method, with a correlation coefficient (R) of 0.9929, indicates that the present procedure can be applied as an alternative to the classic method for determining the AVs of edible oils. PMID:27374571

  4. Spectrophotometric determination of copper(II) in pharmaceutical, biological and water samples by 4-(2'-benzothiazolylazo)-salicylic acid

    Science.gov (United States)

    Hashem, E. Y.; Seleim, M. M.; El-Zohry, A. M.

    2011-09-01

    A highly sensitive method is proposed to determine copper(II) ions by forming a stable complex through their interaction with 4-(2'-benzothiazolylazo)-salicylic acid (BTAS) at room temperature and pH of about 5.0. The complex gave a maximum absorption at λ = 485 nm with a molar absorptivity coefficient of 2.35·104 l/(mol·cm). The linear range for the copper determination is 0.63-5.04 mg/l. The method can be applied to determine copper ions in different biological specimens like some drugs and water samples.

  5. Determination of Arrhenius and Thermodynamic Parameters for the Aqueous Reaction of the Hydroxyl Radical with Lactic Acid

    Energy Technology Data Exchange (ETDEWEB)

    Leigh R. Martin; Stephen P. Mezyk; Bruce J. Mincher

    2009-01-01

    Lactic acid is a major component of the TALSPEAK process planned for use in the separation of trivalent lanthanide and actinide elements. This acid acts both as a buffer, and also to protect the actinide complexant from radiolytic damage. However, there is little kinetic information on the reaction of water radiolysis species with lactic acid, particularly under the anticipated process conditions of aerated aqueous solution at pH~3, where oxidizing reactions are expected to dominate. Here we have determined temperature-dependent reaction rate constants for the reactions of the hydroxyl radical with lactic acid and the lactate ion. For lactic acid this rate constant is given by the equation: ln k1 = (23.85 ± 0.19) – (1120 ± 54) / T, corresponding to an activation energy of 9.31 ± 0.45 kJ mol-1 and a room temperature reaction rate constant of (5.24 ± 0.09) x 108 M-1 s-1 (24.0oC). For the lactate ion, the temperature-dependent rate constant is given by: ln k2 = (24.83 ± 0.14) – (1295 ± 42) / T, for an activation energy of 10.76 ± 0.35 kJ mol-1 and a room temperature value of (7.77 ± 0.11) x 108 M-1 s-1 (22.2oC). These kinetic data have been combined with autotitration measurements to determine the temperature-dependent behavior of the lactic acid pKa value, allowing thermodynamic parameters for the acid dissociation to be calculated as ?Hº = -10.75 ± 1.77 kJ mol-1, ?Sº = -103.9 ± 6.0 J K-1 mol-1 and ?Gº = 20.24 ± 2.52 kJ mol-1 at low ionic strength.

  6. Determination of some hydroxybenzoic acids and catechins in white wine samples by liquid chromatography with luminescence detection.

    Science.gov (United States)

    Rodríguez-Díaz, Rafael Carlos; Paz Aguilar-Caballos, María; Gómez-Hens, Agustina

    2006-12-01

    A liquid chromatographic method with luminescence detection for the determination of eight phenolic compounds is reported. The method involves postcolumn derivatization with terbium(III). This derivatization is based on the reaction between phenolics and terbium(III) to form luminescent chelates, which were determined at lamda ex 295 and lamda em 545 nm using the fluorescence mode. The long wavelength emission of lanthanide chelates can minimize interferences from background sample matrix, which usually emit at shorter wavelengths. Also, the chromatographic separation allows the individual determination of phenolics, which cannot be done using the direct measurement of the fluorescence of their corresponding terbium chelates. Dynamic ranges of the calibration graphs and detection limits, obtained with standard solutions of analytes were (microg/mL): gallic acid (0.9-40, 0.3), protocatechuic acid (0.05-7, 0.016), catechin (0.2-40, 0.07), vanillic acid (0.25-40, 0.08), p-hydroxybenzoic acid (0.8-40, 0.25), syringic acid (0.17-40, 0.05), epicatechin (0.3-40, 0.09) and salicylic acid (0.07-12, 0.02). The precision was established at two concentration levels of each analyte and expressed as the percentage of RSD with values ranging between 1.0 and 6.5%. The practical usefulness of the method was demonstrated by the analysis of white wine samples, which were diluted two-fold and directly injected into the chromatographic system. The recovery values obtained ranged between 93.3 and 108.0%. PMID:17305238

  7. Disposable biosensor based on cathodic electrochemiluminescence of tris(2,2-bipyridine)ruthenium(II) for uric acid determination

    Energy Technology Data Exchange (ETDEWEB)

    Ballesta-Claver, J.; Rodríguez-Gómez, R. [ECsens, Department of Analytical Chemistry, Campus Fuentenueva, Faculty of Sciences, University of Granada, E-18071 Granada (Spain); Capitán-Vallvey, L.F., E-mail: lcapitan@ugr.es [ECsens, Department of Analytical Chemistry, Campus Fuentenueva, Faculty of Sciences, University of Granada, E-18071 Granada (Spain)

    2013-04-03

    Highlights: ► Cathodic ECL offers conventional and non-aggressive analysis conditions. ► The ECL hydrogen peroxide/ruthenium complex system for uric acid determination is novel. ► The ruthenium complex is electrochemically immobilized on graphite screen-printed electrodes. ► The quantification of the uric acid is based on a Stern–Volmer type equation. ► The use of the cathodic ECL working methodology reduces interferences during analysis. -- Abstract: A new method for uric acid (UA) determination based on the quenching of the cathodic ECL of the tris(2,2-bipyridine)ruthenium(II)–uricase system is described. The biosensor is based on a double-layer design containing first tris(2,2-bipyridine)ruthenium(II) (Ru(bpy){sub 3}{sup 2+}) electrochemically immobilized on graphite screen-printed cells and uricase in chitosan as a second layer. The uric acid biosensing is based on the ECL quenching produced by uric acid over the cathodic ECL caused by immobilized Ru(bpy){sub 3}{sup 2+} in the presence of uricase. The use of a −1.1 V pulse for 1 s with a dwelling time of 10 s makes it possible to estimate the initial enzymatic rate, which is used as the analytical signal. The Stern–Volmer type calibration function shows a dynamic range from 1.0 × 10{sup −5} to 1.0 × 10{sup −3} M with a limit of detection of 3.1 × 10{sup −6} M and an accuracy of 13.6% (1.0 × 10{sup −4} M, n = 5) as relative standard deviation. Satisfactory results were obtained for urine samples, creating an affordable alternative for uric acid determination.

  8. Determination of 18 beta-glycyrrhetinic acid in human serum using the fully automated ALCA-system.

    Science.gov (United States)

    Heilmann, P; Heide, J; Schöneshöfer, M

    1997-07-01

    We report a method for the determination of 18 beta-glycyrrhetinic acid (glycyrrhetinic acid) in human serum using the ALCA-system. The technology of the ALCA-system is based on the principles of adsorptive and desorptive processes between liquid and solid phases. The assay is run fully automated and selective. Procedural losses throughout the analysis are negligible, thereby allowing for external calibration. The calibration curve is linear up to 10 mg/l and concentrations as low as 10 micrograms/l are detectable. CV is 2.5% for within- and 7.5% for between-assay precision at a level of 50 micrograms/l and 1.2% for within- and 8.5% for between-assay precision at a level of 500 micrograms/l. Specific and expensive reagents are not necessary and time-consuming manual operations are not involved. This assay can be selected from a wide spectrum of methods at any time. Thus, the present method is well-suited for drug monitoring purposes in the routine laboratory. In a pharmacokinetic study we measured serum levels of glycyrrhetinic acid in ten healthy young volunteers after ingestion of 500 mg glycyrrhetinic acid. Maximum levels of glycyrrhetinic acid were 6.3 mg/l 2 to 4 hours after ingestion. Twenty-four (24) hours after ingestion seven probands still had glycyrrhetinic acid levels above the detection limit with a mean level of 0.33 mg/l.

  9. Critical load of acid precipitations. Mapping of Italian regions; Mappa dei carichi critici di acidita' totale riferita al territorio italiano

    Energy Technology Data Exchange (ETDEWEB)

    Bonanni, P.; Brini, S.; Delmonaco, G.; Liburdi, R.; Trocciola, A.; Vetrella, G. [ENEA Centro Ricerche Casaccia, S. Maria di Galeria, RM (Italy). Dipt. Ambiente

    1999-07-01

    In this report the mapping of critical loads of acidity for the Italian terrestrial ecosystems is presented. The level O method (Stockholm Environment Institute) has been used to determine sensitivity to acid deposition; this semi-quantitative method has been modified to address some Italian characteristics. The results show that the sensitivity of the Italian soils to acidification is not particularly elevated: there are really only few small areas with poor tolerance to acid depositions. These areas are in the north-east of Italy, in Alpine and Prealpine region. [Italian] Nel rapporto vengono riportati i risultati della mappatura, riferita agli ecosistemi terrestri del territorio italiano, dei carichi critici per l'acidita' totale. Il calcolo dei carichi critici e' stato eseguito sulla base della metodologia messa a punto dallo Stokholm Environment Institute; a questo metodo semi-quantitativo sono state apportate alcune modifiche per meglio adattarlo alle caratteristiche del territorio italiano. Dall'analisi dei risultati ottenuti, si evince come la sensibilita' dei suoli italiani all'acidificazione non sia particolarmente elevata: sono state riscontrate infatti solo alcune aree, peraltro con superficie limitata, con una scarsa tolleranza alle deposizioni acide. Tali aree sono localizzate nell'Italia nord-orientale, in zona alpina e prealpina.

  10. 对氯水杨酸的纯度测定%Purity determination of salicylic acid chloride

    Institute of Scientific and Technical Information of China (English)

    杨丰科; 黄震

    2014-01-01

    采用双波长法对对氯水杨酸的纯度进行了测定。对氯水杨酸在乙醇中的最大吸收波长为243 nm,副产物等吸收总波长为267 nm。测定纯对氯水杨酸的标准纯度都超过99.5%,测定市售3种对氯水杨酸的纯度在97.8%~98.0%。研究表明,该方法操作简单,分析数据准确可靠。%Use dual-wavelength method to determine the purity of p-chlorine salicylic acid. The maximum absorption wavelength of p-chlorine salicylic acid in ethanol is 243 nm. The total absorption wavelength of byproducts is 267 nm. Determination of the standard purity of pure p-chlorine salicylic acid more than 99 . 5%. Determination of the purity of three kinds of commercially available p-chlorine salicylic acid was 97. 8 % ~98. 0 %. Studies show that the method is simple,the analytical data is accurate and reliable.

  11. Determination of Amino Acids in Panax notoginseng by Microwave Hydrolysis and Derivatization Coupled with Capillary Zone Electrophoresis Detection

    Institute of Scientific and Technical Information of China (English)

    LI Xiao-tian; ZHAO Ya-jing; JIANG Cheng-fei; ZHANG Han-qi; YU Ai-min

    2013-01-01

    The microwave hydrolysis and derivatization coupled with capillary electrophoresis detection were developed for the separation and determination of the amino acids in Panax notoginseng.The experimental conditions for the microwave hydrolysis and derivatization were examined and optimized.Several parameters of capillary electrophoresis,such as pH value of background electrolyte,borate concentration and applied voltage were optimized.Under the selected conditions,11 amino acids were completely separated.The real sample was analyzed and the results were satisfactory.Compared with that of conventional heat hydrolysis and derivatization,the analytical time of this method was significantly shortened.

  12. Determination of effect factor for effective parameter on saccharification of lignocellulosic material by concentrated acid

    Science.gov (United States)

    Aghili, Sina; Nodeh, Ali Arasteh

    2015-12-01

    Tamarisk usage as a new group of lignocelluloses material to produce fermentable sugars in bio ethanol process was studied. The overall aim of this work was to establish the optimum condition for acid hydrolysis of this new material and a mathematical model predicting glucose release as a function of operation variable. Sulfuric acid concentration in the range of 20 to 60%(w/w), process temperature between 60 to 95oC, hydrolysis time from 120 to 240 min and solid content 5,10,15%(w/w) were used as hydrolysis conditions. HPLC was used to analysis of the product. This analysis indicated that glucose was the main fermentable sugar and was increase with time, temperature and solid content and acid concentration was a parabola influence in glucose production. The process was modeled by a quadratic equation. Curve study and model were found that 42% acid concentration, 15 % solid content and 90oC were optimum condition.

  13. Determination of Uranyl Nitrate and Nitric Acid Based on Density and Conductivity Measurements

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    <正>Measurement of the uranium and acidity plays an important role in process control of spent fuel reprocessing. The main chemical compositions including a mount of U solution in spent fuel reprocessing

  14. Impedimetric test for rapid determination of performic acid (PFA) biocidal activity toward Echerichia coli

    OpenAIRE

    Małgorzata Lasik; Renata Dobrucka; Piotr Konieczny

    2013-01-01

      Background. Performic acid has recently become available on a commercial scale for potential use in waste-water disinfection and can become an innovative biocide for various purposes in food processing. The aim of our study was: 1) to investigate the antimicrobial resistance of performic acid as high active and non toxic chemical disinfectant against Escherichi coli (hygiene indicator test  microorganism used in industrial micro- biology) and 2) to evaluate the electrical impedanc...

  15. Simultaneous determination of B-vitamins and ascorbic acid in multi-vitamin preparations by reversed-phase HPLC.

    Science.gov (United States)

    Tee, E S; Khor, S

    1996-09-01

    The tedious and time consuming methods employed for the analysis of individual B-vitamins can now be replaced by ion-pair reversed-phase high-performance liquid chromatographic (HPLC) methods. This laboratory has previously reported the simultaneous determination of eight water-soluble vitamin standards that is, B1, B2, B6, B12, C, niacin, niacinamide and folic acid. The proposed isocratic HPLC method, employing 3 channels of detection, adequately separated all eight vitamins in less than 20 minutes. This study reports another phase of the project whereby the method was employed for the analysis of pharmaceutical preparations. Different extraction procedures were first evaluated, namely acid, acid plus enzyme and alkaline hydrolysis methods, using vitamin standards, individual vitamin tablets and multivitamin preparations. The amounts obtained from the analysis were compared with the declared values. Recovery studies were also carried out. The method of acid hydrolysis with 0.1N sulphuric acid was found suitable for use and was thus adopted as the extraction procedure for the analysis of 10 multivitamin preparations obtained from various pharmaceutical outlets. For most of these preparations, the amount obtained were close to the declared values, except for folic acid and cyanocobalamin. Further trials on folic acid showed that the problem could be resolved by omitting the filtration step in the final extract after acid hydrolysis and diluting with 0.01N sodium hydroxide before processing for chromatography. Vitamin B12 was not detectable using the present chromatography system probably because of its low concentration in the samples studied. PMID:22692140

  16. Determination of cholesterol oxides in anchovies (Engraulis encrasicolus treated with a commercial mixture of citric acid, trisodium acid and hydrogen peroxide

    Directory of Open Access Journals (Sweden)

    Aniello Anastasio

    2013-02-01

    Full Text Available A new additive formulation containing hydrogen peroxide, citric acid and trisodium acid is illegally used in fishery products due its whitening and antioxidant features. Aim of this study was to evaluate the possible presence of COPs and their role as markers of illegal treatment in anchovies (Engraulis encrasicolus stored at different temperatures. Sensory analysis was also performed by the specific QIM test. The quantitative determinations (% of cholesterol oxides (COPs showed changing amounts during storage. Not always The COPs measured in the treated samples were significantly higher than control samples. Considering the volatility of hydrogen peroxide and the poor repeatability of COPs analyses, as shown in the present study, it is crucial to intensify the control by the Authorities.

  17. 离子色谱法测定工业废气中的甲酸、乙酸和丙酸%Industrial waste gas by ion chromatography determination of formic acid, acetic acid and propionic acid

    Institute of Scientific and Technical Information of China (English)

    吴红星

    2013-01-01

    建立了用离子色谱法测定工业废气中甲酸、乙酸和丙酸的新方法,常规无机阴离子对本方法的测定没有干扰。本方法分析速度快,所需样品量少,且无需要复杂的前处理,简便、灵敏、可靠。%established by ion chromatography determination of formic acid , acetic acid and propionic acid in industrial waste gas , a new method for the determination of inorganic anions , the conventional method without interference .This method is fast , small quantity of sam-ple, and no need of complicated pretreatment , simple, sensitive, reliable.

  18. Break Even Price. Un nuovo metodo di definizione del prezzo per l’impresa culturale

    Directory of Open Access Journals (Sweden)

    Fabiana Sciarelli

    2015-12-01

    Full Text Available Nel caso delle imprese che producono servizi per la società, come quelle culturali, l’obiettivo primario è la diffusione del servizio per un miglioramento della società stessa. Per aumentare la diffusione della cultura, le imprese devono applicare prezzi bassi, ma per evitare squilibri economici, devono necessariamente accedere a finanziamenti pubblici o privati, che in questo lavoro chiameremo ricavi fissi. Molte imprese culturali hanno, inoltre, vincoli strutturali, come ad esempio i posti agibili di un teatro, che determinano la quantità massima producibile e vendibile. Per raggiungere l’equilibrio economico, quindi, un’impresa culturale, non avendo la compiuta possibilità di variare la quantità prodotta e venduta, non potendo ridurre i costi senza modificare la qualità del servizio, ha una principale variabile di intervento: il prezzo. Il prezzo diviene, infatti, una variabile strategica che i metodi tradizionali di determinazione dello stesso non sono atti a definire. In particolare il metodo basato sui costi risulta inadeguato non considerando i ricavi fissi e quindi la parziale copertura dei costi stessi attraverso i finanziamenti. Le caratteristiche dell’impresa artistico-culturale, nonché la conseguente inadeguatezza dei tradizionali metodi di definizione del prezzo, ci indirizzano ad utilizzare il BEP come la base teorica di un innovativo sistema di definizione del prezzo di equilibrio (Break Even Price, ossia del prezzo più basso che l’impresa può far pagare al fruitore per recuperare i costi totali, realizzare la propria mission e sopravvivere.   In cultural companies, and in particular in those producing services for the society, the main goal is spreading the service to improve community. In these cases, prices for services are fundamental elements to achieve the mission itself. To increase their services, these companies must often apply low prices, but to avoid economic imbalance, they must necessarily access

  19. Field turbidity method for the determination of lead in acid extracts of dried paint.

    Science.gov (United States)

    Studabaker, William B; McCombs, Michelle; Sorrell, Kristen; Salmons, Cynthia; Brown, G Gordon; Binstock, David; Gutknecht, William F; Harper, Sharon L

    2010-07-01

    Lead, which can be found in old paint, soil, and dust, has been clearly shown to have adverse health effects on the neurological systems of both children and adults. As part of an ongoing effort to reduce childhood lead poisoning, the US Environmental Protection Agency promulgated the Lead Renovation, Repair, and Painting Program (RRP) rule requiring that paint in target housing built prior to 1978 be tested for lead before any renovation, repair, or painting activities are initiated. This rule has led to a need for a rapid, relatively easy, and an inexpensive method for measuring lead in paint. This paper presents a new method for measuring lead extracted from paint that is based on turbidimetry. This method is applicable to paint that has been collected from a surface and extracted into 25% (v/v) of nitric acid. An aliquot of the filtered extract is mixed with an aliquot of solid potassium molybdate in 1 M ammonium acetate to form a turbid suspension of lead molybdate. The lead concentration is determined using a portable turbidity meter. This turbidimetric method has a response of approximately 0.9 NTU per microg lead per mL extract, with a range of 1-1000 Nephelometric Turbidity Units (NTUs). Precision at a concentration corresponding to the EPA-mandated decision point of 1 mg of lead per cm(2) is measurement using the new turbidimetric method, and the other half was analyzed using microwave extraction and measurement by ICP-AES. The average relative percent difference between the turbidimetric method and the ICP-AES method for the 24 sets measured as milligrams of lead per cm(2) is -0.63 +/- 32.5%; the mean difference is -2.1 +/- 7.0 mg lead per cm(2). Non-parametric and parametric statistical tests on these data showed no difference in the results for the two procedures. At the federal regulated level of 1 mg of lead per cm(2) paint, this turbidimetric method meets the performance requirements for EPA's National Lead Laboratory Accreditation Program (NLLAP

  20. Sensitive determination of dopamine in the presence of uric acid and ascorbic acid using TiO2 nanotubes modified with Pd, Pt and Au nanoparticles.

    Science.gov (United States)

    Mahshid, Sara; Li, Chengcheng; Mahshid, Sahar Sadat; Askari, Masoud; Dolati, Abolghasem; Yang, Lixia; Luo, Shenglian; Cai, Qingyun

    2011-06-01

    A simple modified TiO(2) nanotubes electrode was fabricated by electrodeposition of Pd, Pt and Au nanoparticles. The TiO(2) nanotubes electrode was prepared using the anodizing method, followed by modifying Pd nanoparticles onto the tubes surface, offering a uniform conductive surface for electrodeposition of Pt and Au. The performance of the modified electrode was characterized by cyclic voltammetry and differential pulse voltammetry methods. The Au/Pt/Pd/TiO(2) NTs modified electrode represented a high sensitivity towards individual detection of dopamine as well as simultaneous detection of dopamine and uric acid using 0.1 M phosphate buffer solution (pH 7.00) as the base solution. In both case, electro-oxidation peak currents of dopamine were linearly related to accumulated concentration over a wide concentration range of 5.0 × 10(-8) to 3.0 × 10(-5) M. However in the same range of dopamine concentration, the sensitivity had a significant loss at Pt/Pd/TiO(2) NTs electrode, suggesting the necessity for Au nanoparticles in modified electrode. The limit of the detection was determined as 3 × 10(-8) M for dopamine at signal-to-noise ratio equal to 3. Furthermore, the Au/Pt/Pd/TiO(2) NTs modified electrode was able to distinguish the oxidation response of dopamine, uric acid and ascorbic acid in mixture solution of different acidity. It was shown that the modified electrode possessed a very good reproducibility and long-term stability. The method was also successfully applied for determination of DA in human urine samples with satisfactory results. PMID:21494708

  1. Expansion 5-6 of heterocyclic compounds by Stork-De Selms method; Expansion 5-6 de compuestos heterociclicos por el metodo de Stork-De Selms

    Energy Technology Data Exchange (ETDEWEB)

    Albores, Marta E.; Maldonado, Luis A. [Universidad Nacional Autonoma de Mexico, Mexico, D.F. (Mexico)

    1999-08-01

    The construction of the chromone, thiochromone and 4-quinolone ring systems by ring expansion of appropriate 5-membered heterocyclic enol acetates, with dibromocarbene generated by Seyferth's method, is described. The use of the method for the synthesis of 2-bromo-1-naphthyl acetate and an attempted synthesis of the flavone ring are also reported. [Spanish] Se describe la construccion de los sistemas anulares de cromona, tiocromona y 4-quinolona por la expansion de acetatos de enol heterociclicos apropiados, con dibromocarbeno generado por el metodo de Seyferth. Tambien se informa del uso de este metodo para la sintesis del acetato de 2-bromo-1-naftilo y del intento de sintesis del anillo de flavona.

  2. A method for the optimal design of networks of drinking water distribution; Un metodo para el diseno optimo de redes de distribucion de agua potable

    Energy Technology Data Exchange (ETDEWEB)

    Fuentes Mariles, O. A.; Carrillo Sosa, J.J. [Instituto de Ingenieria, UNAM, Mexico, D.F. (Mexico)

    1998-12-01

    A method to select, among several commercial diameter options, the most economic combination of pipeline networks is presented. These networks comply with the discharge conditions in the pipes and pressure in the knots. It is applied a static method for the hydraulics analysis of the Engineering Institute of the Universidad Nacional Autonoma de Mexico (UNAM) and an optimization technique to reduce the number of calculations. [Spanish] Se presenta un metodo para seleccionar, de entre varias opciones de diametros comerciales, la combinacion que forma la red de tuberias mas economica que satisface las condiciones de gasto en los tubos y de presion en los nudos de la misma. Para el analisis hidraulico se emplea un metodo estatico del Instituto de Ingenieria de la Universidad Nacional Autonoma de Mexico (UNAM) y se aplica una tecnica de optimacion para reducir el numero de calculos y alcanzar la solucion.

  3. A method for the optimum design of drinking water distribution networks; Un metodo para el diseno optimo de redes de distribucion de agua potable

    Energy Technology Data Exchange (ETDEWEB)

    Fuentes Mariles, O. A.; Carrillo Sosa, J. J. [Universidad Nacional Autonoma de Mexico, Mexico, D.F. (Mexico)

    1998-12-01

    A method to select, among several commercial diameter options, the most economic combination of pipeline networks is presented. These networks comply with the discharge conditions in the pipes and pressure in the knot. It is applied a static method for the hydraulics analysis and an optimisation technique to reduce the number of calculations. [Spanish] Se presenta un metodo para seleccionar, de entre varias opciones de diametros comerciales, la combinacion que forma la red de tuberias mas economicas que satisface las condiciones de gasto en los tubos y de presion en los nudos de la misma. Para el analisis hidraulico se emplea un metodo estatico del Instituto de Ingenieria, UNAM y se aplica una tecnica de optimacion para reducir el numero de calculos y alcanzar la solucion.

  4. Application of neutron activation analysis to the determination of total mercury and other elements of interest in soil and sediment samples from Serra do Navio and Vila Nova River Basin, Amapa, Brazil; Aplicacao do metodo de ativacao neutronica a determinacao do mercurio total e outros elementos de interesse em amostras de solo e sedimento da Serra do Navio e Bacia do Rio Vila Nova, Amapa

    Energy Technology Data Exchange (ETDEWEB)

    Goncalves, Cristina

    1997-07-01

    In this work it is presented a survey on total mercury determination by a radiochemical method in sediment and soil samples from two regions, in the state of Amapa: Serra do Navio (background area) and Vila Nova river basin (gold mining area). The method consisted in leaching of the irradiated samples with acqua regia in a Parr bomb, and heating in microwave oven, for one minute. Then the solvent extraction technique was applied, using bismuth diethyldithiocarbamate (Bi(DDC){sub 3}) as extractant agent. The organic phase, containing {sup 197}Hg and {sup 203}Hg radioisotopes, was measured in a gamma spectrometer with hyper pure Ge detector. This method eliminated the interference of the 279.54 keV photopeak of {sup 75}Se on 279.2 keV photopeak of {sup 203}Hg, besides improving counting statistics of both Hg radioisotopes. The elements As, Ba, Br, Ce, Co, Cr, Cs, Eu, Fe, Hf, Ho, K, La, Lu, Mg, Mn, Na, Nd, Rb, Sb, Sc, Se, Sm, Ta, Tb, Th, Ti, U, V, W, Yb, Zn and Zr were also determined by the instrumental neutron activation analysis. Two irradiation series were carried out to quantify these elements in soil and sediment samples; a short term irradiation allowed to evaluate Mg, Mn, Na, Ti and V levels, and by long term irradiation, the other elements were determined. Precision and accuracy of radiochemical procedure were verified by means of analysis of the reference materials Buffalo River Sediment and Lake Sediment, for sediments and GXR-5, for soils. For the instrumental analysis, the reference materials Buffalo River Sediment, Soil 7, JB-1 and Oyster Tissue were used. The samples were also submitted to X ray diffraction, in Instituto de Geoscience-USP, to observe mercury behaviour with mineralogy. Aluminium concentration was determined by X ray fluorescence method, in the Department of Materials, IPEN/CNEN-SP, making possible enrichment factor calculation so that mercurial contamination in the gold mining area (Vila Nova river basin) could be evaluated. The mercury

  5. Kinetic Spectrophotometric Determination of Trace Titanium(Ⅳ) Based on Oxidation Discoloration of Acid Chrome Blue K with Hydrogen Peroxide

    Institute of Scientific and Technical Information of China (English)

    XIONG Yan; ZHOU Zhi-rong; WU Fu-hai

    2007-01-01

    A simple and sensitive kinetic spectrophotometric method for the determination of trace amounts of titanium(IV), based upon the catalytic effect of Ti(IV) on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid, is described. The reaction rate is monitored spectrophotometrically by measuring the decrease in absorbance of ACBK at 524 nm. The detection limit of the method is 1.01×10-9 g/mL, and the linear range is 0-0.048 mg/L. The influence of acidity, concentration of reactants, reaction time, reaction temperature and for-eign ions is also discussed. The optimum reaction conditions were established and some kinetic parameters determined. The apparent activation energy of the catalytic reaction is 5.32 kJ/mol. The relative standard deviation for the determi-nation of titanium(IV) at the concentration of 0.048 mg/L is calculated to be 1.31% (n = 11). In combination with sol-vent extraction separation, the method has been successfully applied to the determination of trace titanium(IV) in human hair, plant matter, tea and rock samples. The results are in good agreement with the certified values with the relative standard deviations (RSD) of 1.4%-3.5%.

  6. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ying; Shi, Zeming; Zong, Qinxia; Wu, Peng; Su, Jing [Sichuan Provincial Key Laboratory of Nuclear Technology in Geology, College of Nuclear Technology and Automation Engineering, Chengdu University of Technology, Chengdu 610059 (China); Liu, Rui, E-mail: liur.ray@gmail.com [Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059 (China)

    2014-02-17

    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched {sup 201}Hg isotopic spike is added to cosmetics and the isotope ratios of {sup 201}Hg/{sup 202}Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL{sup −1}. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method.

  7. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched 201Hg isotopic spike is added to cosmetics and the isotope ratios of 201Hg/202Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL−1. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method

  8. Quantitative determination of amorphous nicardipine hydrochloride in long acting formula (NIC-LA) using light anhydrous silicic acid.

    Science.gov (United States)

    Kohinata, Takeru; Fujii, Mitsuo; Nakamura, Souichiro; Hamada, Noritaka; Yonemochi, Etsuo; Terada, Katsuhide

    2004-12-01

    We investigated a method to quantitatively determine amorphous nicardipine hydrochloride (NIC) in the NIC-long acting formula (LA) model formulas prepared using NIC, light anhydrous silicic acid (LASA) and carboxymethylethylcellulose (CMEC). Consequently, since the quantity of total NIC in the formula can be determined by means of HPLC and crystal NIC can be determined by the differential scanning calorimetry (DSC) method because the heat of fusion (85.08 J/g) of NIC is constant and unaffected by excipients, we developed the HPLC-DSC method by which the quantity of amorphous NIC is calculated as the difference between the quantity of total NIC determined by HPLC and the quantity of crystal NIC determined by DSC. This practical HPLC-DSC method was confirmed to have good accuracy and reproducibility.

  9. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L-Cysteine in real samples using quercetin silver nanoparticles-graphene nanosheets modified glassy carbon electrode

    Science.gov (United States)

    Zare, Hamid R.; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-07-01

    By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q-AgNPs-GNs-GCE) a new sensor has been fabricated. The cyclic voltammogram of Q-AgNPs-GNs-GCE shows a stable redox couple with surface confined characteristics. Q-AgNPs-GNs-GCE demonstrated a high catalytic activity for L-Cysteine (L-Cys) oxidation. Results indicated that L-Cys peak potential at Q-AgNPs-GNs-GCE shifted to less positive values compared to GNs-GCE or AgNPs-GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k‧, for the oxidation of L-Cys at the Q-AgNPs-GNs-GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L-Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9-12.4 μM and 12.4-538.5 μM of L-Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L-Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L-Cys in a milk sample and UA in a human urine sample.

  10. Determination of Critical Point of pO2 Level in the Production of Lactic Acid by Lactobacillus rhamnosus

    Science.gov (United States)

    Mel, Maizirwan; Karim, Mohamed Ismail Abdul; Salleh, Mohamad Ramlan Mohamed; Abdullah, Rohane

    The study was conducted to determine the critical point of pO2 level in the production of lactic acid by Lactobacillus rhamnosus. The fermentation process was successfully carried out in laboratory scale fermenter/bioreactor using different pO2 level (the main parameter that significantly affects the growth of L. rhamnosus and lactic acid production) together with two other parameters; the agitation rate and pH. From the result, it was observed that the best production of lactic acid with the concentration of 16.85 g L-1 or 1.68% production yield has been obtained at the operating parameters of 5% pO2 level, agitation speed of 100 rpm and sample pH 6. The critical point of pO2 was found to be between 5 and 10%.

  11. Direct Spectroscopic Determination of Europium(Ⅱ) Concentration During Europium(Ⅲ) Electro-Reduction in Hydrochloric Acid Medium

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    UV-Vis spectroscopy was used to directly determine the concentration of Eu(Ⅱ) during electroreduction of Eu(Ⅲ) in hydrochloric acid medium. Electroreduction was carried out in a flow type electrolyzer with glassy carbon cathode at the constant potential of -800 mV vs. Ag/AgCl. The effects of oxygen and concentration of hydrochloric acid on the system were investigated. For 0.01 mol·L-1 hydrochloric acid, calibration curves for Eu(Ⅱ) absorption bands at 248 and 320 nm were constructed. Molar absorption coefficients were estimated to be 2016 and 648 L·mol-1·cm-1, respectively. The absorbance strongly decreased with decrease in pH of the solution, whereas concentration of chloride had only a negligible effect.

  12. Determination of α-Linoleic Acid, Linoleic Acid and Oleic Acid in Hemp Seed by HPLC%HPLC同时测定火麻仁中α-亚麻酸、亚油酸和油酸含量

    Institute of Scientific and Technical Information of China (English)

    秦建平; 陆艳芹; 罗雪磊; 吴建雄; 李家春; 萧伟

    2012-01-01

    目的:建立同时测定火麻仁中的α-亚麻酸、亚油酸和油酸含量的HPLC方法.方法:色谱柱为Kromasil 100-5 C18(4.6 mm×250 mm,5 μm),以乙腈-o.1%磷酸(80∶20)为流动相,流速1 mL? min-1,柱温30℃,检测波长203 nm.结果:α-亚麻酸在34.625~554 mg? L-1(r=0.999 9),亚油酸在56.375~902 mg?L -1(r=1),油酸在17.125 ~ 274 mg? L-1(r =0.999 9)呈良好的线性关系;平均回收率α-亚麻酸为96.38%,RSD0.93%(n=6);亚油酸为97.79%,RSD 0.92%(n=6);油酸为97.06%,RSD 1.51% (n =6).结论:本法简便准确,专属性强,重复性好,可作为火麻仁的质量控制的参考.%Objective: To establish a HPLC method for the determination of a-linoleic acid, linoleic acid and oleic acid in Hemp Seed. Method; The Kromasil 100-5 C18 (4.6 mm ×250 mm, 5 μm) column was used with a mobile phase of acetonitrile-0. 1% phosphoric acid (80:20) , the flow rate was 1 mL ? Min-1 , the column temperature was at 30 ℃, the detection wavelength was at 203 nm. Result: The linear ranges of a-linoleic acid, linoleic acid and oleic acid were 34. 625-554 mg ? L-1 ( r = 0. 999 9) , 56. 375-902 mg ? L-1 ( r = 1 ) and 17. 125-274 mg ? L-1 (r=0. 999 9) respectively. The average recoveries were 96. 38% with RSD 0. 93% for a-linoleic acid, 97. 79% with RSD 0. 92% for linoleic acid, 97. 06% with RSD 1. 51% for oleic acid. Conclusion; The method can be used to control the quality of a-linoleic acid, linoleic acid and oleic acid in Hemp Seed, which is simple, accurate, convenient, specific and repeatable.

  13. Method to allow the estimation of heat transfer coefficients in solar stills; Metodo para determinar coeficientes locales de transferencia de calor en destiladores solares

    Energy Technology Data Exchange (ETDEWEB)

    Rubio Cerda, Eduardo; Porta Gandara, Miguel A [CIBNOR, Mexico D.F (Mexico); Fernandez Zayas, Jose Luis [UNAM Mexico, D.F. (Mexico)

    2000-07-01

    This work reports an experimental method that allows to estimate the heat transfer coefficients in the neighborhood of walls or flat plates subject to convective transport phenomena. This method can be applied to a great variety of thermal systems since it is based on the knowledge of the border condition for the temperature at the surface of the plate, and the temperature profile that characterize the dimensionless coefficient of heat transfer in the fluid, according to its definition given by the Nusselt number. The approach of this work are the foundations of the method and the system that has been developed to apply it, that incorporates automatic acquisition equipment for continuos monitoring of the information and elements to control the parameters of interest. In addition, the experimental cavities on which the method will be evaluated are discussed, considering two different scales, as well as experiments in cavities filled with air, and with a mixture of air and steam water, as is the case for solar distillation. [Spanish] En este trabajo se presenta un metodo que permite determinar de manera experimental coeficientes de transferencia de calor por conveccion. Este metodo puede ser aplicado a una gran variedad de sistemas termicos ya que se fundamenta en el conocimiento de la condicion de frontera para la temperatura en la superficie de la placa, y del perfil de temperaturas que caracteriza el coeficiente adimensional de transferencia de calor en el fluido, de acuerdo a la definicion de este, dada por el numero de Nusselt. El trabajo que aqui se reporta esta enfocado a la fundamentacion del metodo y al equipamiento que se ha desarrollado para instrumentarlo, que incorpora equipos automaticos de adquisicion continua de informacion y elementos de control para los parametros de interes. Se presentan ademas, las cavidades experimentales sobre las que sera evaluado el metodo, que considera dos escalas diferentes, asi como experimentos en cavidades llenas de aire

  14. ANALISI DELLA COMUNICAZIONE TRA PEDIATRA E MADRE ATTRAVERSO L'APPLICAZIONE DEL METODO F.A.C.S. DI P. EKMAN E W.V. FRIESEN

    OpenAIRE

    GRECO, VANESSA

    2007-01-01

    ABSTRACT In questo nostro lavoro abbiamo analizzato il rapporto pediatra – madre e bambino partendo dalla letteratura relativa a questo argomento, che ha avuto un particolare sviluppo negli anni successivi al 1960. L’originalità del nostro progetto consiste nell’aver utilizzato il sistema F.A.C.S – Facial Action Coding System - di P. Ekman e W. V. Friesen. Tale metodo consiste nella decodificazione delle espressioni emozionali del volto, quali sorpresa, paura, collera, disgusto, tristezz...

  15. A new approach for noninvasive transdermal determination of blood uric acid levels

    Directory of Open Access Journals (Sweden)

    Ching CTS

    2014-06-01

    Full Text Available Congo Tak-Shing Ching,1,2 Kok-Khun Yong,3 Yan-Dong Yao,4 Huan-Ting Shen,3 Shiu-Man Hsieh,5 Deng-Yun Jheng,1 Tai-Ping Sun,1,6 Hsiu-Li Shieh11Department of Electrical Engineering, National Chi Nan University, Nantou, 2Department of Photonics and Communication Engineering, Asia University, Taichung, 3Department of Internal Medicine, Puli Christian Hospital, Nantou, People’s Republic of China; 4Division of Science and Technology, Hong Kong Community College, Hong Kong; 5Department of Orthopedic Surgery, Puli Christian Hospital, 6Department of Electronic Engineering, Nan Kai University of Technology, Nantou, People’s Republic of ChinaAbstract: The aims of this study were to investigate the most effective combination of physical forces from laser, electroporation, and reverse iontophoresis for noninvasive transdermal extraction of uric acid, and to develop a highly sensitive uric acid biosensor (UAB for quantifying the uric acid extracted. It is believed that the combination of these physical forces has additional benefits for extraction of molecules other than uric acid from human skin. A diffusion cell with porcine skin was used to investigate the most effective combination of these physical forces. UABs coated with ZnO2 nanoparticles and constructed in an array configuration were developed in this study. The results showed that a combination of laser (0.7 W, electroporation (100 V/cm2, and reverse iontophoresis (0.5 mA/cm2 was the most effective and significantly enhanced transdermal extraction of uric acid. A custom-designed UAB coated with ZnO2 nanoparticles and constructed in a 1×3 array configuration (UAB-1×3-ZnO2 demonstrated enough sensitivity (9.4 µA/mM for quantifying uric acid extracted by the combined physical forces of laser, electroporation, and RI. A good linear relationship (R2=0.894 was demonstrated to exist between the concentration of uric acid (0.2–0.8 mM inside the diffusion cell and the current response of the

  16. Determination of free fatty acids in olive oils by UPHLC-MS.

    Science.gov (United States)

    Wabaidur, Saikh M; AlAmmari, Ahmad; Aqel, Ahmad; Al-Tamrah, Saad A; Alothman, Zeid Abdullah; Ahmed, A Y Badjah Hadj

    2016-09-15

    A simple, fast, highly efficient and direct method using ultra-performance liquid chromatography coupled to mass spectrometry has been established for the simultaneous separation, identification and quantitation of a few saturated and unsaturated fatty acids in olive oils from various countries. No sample pretreatment techniques were employed such as extraction or derivatization for the analysis of target acids from oil samples, as the oil samples were just diluted, filtered and then directly injected to the instrument. The chromatographic separations of all target fatty acids were achieved on a Hypersil Gold C18 column of particle size 1.9μm, 50×2.1mm I.D, while the gradient elution using a binary mobile phase mixture of acetonitrile and water at a flow rate of 1.5ml/min was adopted for achieving optimum separations. The identification and quantitation of target compounds was accomplished using selected ion reaction monitoring mode. The recoveries of the fatty acids were obtained higher than 89% with good validation parameters; linearity (r(2)>0.992), detection limit between 0.09 and 0.24μg/ml, run to run and day to day precisions with percent relative standard deviation lower than 2.4% at both low (1μg/ml) and medium (10μg/ml) concentration levels. The total content of fatty acids in each individual oils was found in the range of 472.63-7751.20μg/ml of olive oil, while oleic acid was found to be the major fatty acid among all analyzed oils with the amount 3785.94μg/ml (maximum) in Syrian olive oil. The obtained validation parameters confirm that the proposed analytical method is rapid, sensitive, reproducible and simple and it could be applied for the successful evaluation of fatty acids in various oils and other matrices. All the fatty acids were efficiently eluted in a time of less than 8min with well resolved peaks by employing the proposed method. PMID:27474779

  17. Role of enthalpy-entropy compensation interactions in determining the conformational propensities of amino acid residues in unfolded peptides.

    Science.gov (United States)

    Toal, Siobhan E; Verbaro, Daniel J; Schweitzer-Stenner, Reinhard

    2014-02-01

    The driving forces governing the unique and restricted conformational preferences of amino acid residues in the unfolded state are still not well understood. In this study, we experimentally determine the individual thermodynamic components underlying intrinsic conformational propensities of these residues. Thermodynamic analysis of ultraviolet-circular dichroism (UV-CD) and (1)H NMR data for a series of glycine capped amino acid residues (i.e., G-x-G peptides) reveals the existence of a nearly exact enthalpy-entropy compensation for the polyproline II-β strand equilibrium for all investigated residues. The respective ΔHβ, ΔSβ values exhibit a nearly perfect linear relationship with an apparent compensation temperature of 295 ± 2 K. Moreover, we identified iso-equilibrium points for two subsets of residues at 297 and 305 K. Thus, our data suggest that within this temperature regime, which is only slightly below physiological temperatures, the conformational ensembles of amino acid residues in the unfolded state differ solely with respect to their capability to adopt turn-like conformations. Such iso-equilibria are rarely observed, and their existence herein indicates a common physical origin behind conformational preferences, which we are able to assign to side-chain dependent backbone solvation. Conformational effects such as differences between the number of sterically allowed side chain rotamers can contribute to enthalpy and entropy but not to the Gibbs energy associated with conformational preferences. Interestingly, we found that alanine, aspartic acid, and threonine are the only residues which do not share these iso-equilbiria. The enthalpy-entropy compensation discovered as well as the iso-equilbrium and thermodynamics obtained for each amino acid residue provide a new and informative way of identifying the determinants of amino acid propensities in unfolded and disordered states.

  18. Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Yang Guangming, E-mail: yangguangmingbs@126.com [Department of Resources and Environment, Baoshan University, Baoshan 678000 (China); Li Ling [Department of Resources and Environment, Baoshan University, Baoshan 678000 (China); Jiang Jinhe; Yang Yunhui [College of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming 650092 (China)

    2012-08-01

    Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02 Multiplication-Sign 10{sup -7}-5.23 Multiplication-Sign 10{sup -4} mol L{sup -1} and 1.43 Multiplication-Sign 10{sup -7}-4.64 Multiplication-Sign 10{sup -4} mol L{sup -1}, the detection limits were 1.12 Multiplication-Sign 10{sup -8} mol L{sup -1} and 2.24 Multiplication-Sign 10{sup -8} mol L{sup -1}, respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. - Graphical abstract: The schematic diagram of formation of Au nanotube arrays (a) and the stepwise procedure of the sensor (b). Highlights: Black-Right-Pointing-Pointer Gold nanotubes array has been synthesized by cyclic voltammetry. Black-Right-Pointing-Pointer The mechanism of deposition of gold nanotube has been discussed. Black-Right-Pointing-Pointer A determination of ascorbic acid and uric acid was constructed by gold array. Black-Right-Pointing-Pointer A satisfied determination of samples can be obtained by this sensor.

  19. GC-based detection of aldononitrile acetate derivatized glucosamine and muramic acid for microbial residue determination in soil.

    Science.gov (United States)

    Liang, Chao; Read, Harry W; Balser, Teri C

    2012-01-01

    Quantitative approaches to characterizing microorganisms are crucial for a broader understanding of the microbial status and function within ecosystems. Current strategies for microbial analysis include both traditional laboratory culture-dependent techniques and those based on direct extraction and determination of certain biomarkers. Few among the diversity of microbial species inhabiting soil can be cultured, so culture-dependent methods introduce significant biases, a limitation absent in biomarker analysis. The glucosamine, mannosamine, galactosamine and muramic acid have been well served as measures of both the living and dead microbial mass, of these the glucosamine (most abundant) and muramic acid (uniquely from bacterial cell) are most important constituents in the soil systems. However, the lack of knowledge on the analysis restricts the wide popularization among scientific peers. Among all existing analytical methods, derivatization to aldononitrile acetates followed by GC-based analysis has emerged as a good option with respect to optimally balancing precision, sensitivity, simplicity, good chromatographic separation, and stability upon sample storage. Here, we present a detailed protocol for a reliable and relatively simple analysis of glucosamine and muramic acid from soil after their conversion to aldononitrile acetates. The protocol mainly comprises four steps: acid digestion, sample purification, derivatization and GC determination. The step-by-step procedure is modified according to former publications. In addition, we present a strategy to structurally validate the molecular ion of the derivative and its ion fragments formed upon electron ionization. We applied GC-EI-MS-SIM, LC-ESI-TOF-MS and isotopically labeled reagents to determine the molecular weight of aldononitrile acetate derivatized glucosamine and muramic acid; we used the mass shift of isotope-labeled derivatives in the ion spectrum to investigate ion fragments of each derivatives. In

  20. Determination of the oxygen-18/oxygen-16 isotope ratios of sugar, citric acid and water from single strength orange juice.

    Science.gov (United States)

    Houerou, G; Kelly, S D; Dennis, M J

    1999-01-01

    The ratio of the stable isotopes of oxygen (18O/16O) has been measured in the sugar, citric acid and water from authentic single strength orange juices, originating from a number of different countries. The sugars and citric acid were recovered from the juices and their 18O/16O ratios were determined by pyrolysis/continuous flow-isotope ratio mass spectrometry (Py/CF-IRMS). The 18O/16O ratio of the fruit juice water was determined by the carbon dioxide/water equilibration method. The delta 18O/1000 values of 45 different sugars ranged from +29.1 to +38.8/1000 and 15 citric acids ranged from +18.9 to +25.4/1000. The delta 18O/1000 value of the water present in the same samples ranged from -2.1 to +7.8/1000. A correlation was evident between the delta 18O/1000 values of the sugar, citric acid and water from the juices. This information can be used to improve the assessment of the authenticity of commercial 'freshly squeezed' orange juices. The detection of the presence of reconstituted orange juice concentrate in 'freshly squeezed' orange juices was improved by 37% using regression analysis of the combined water and sugar delta 18O/1000 ratios when compared to the use of delta 18O/1000 ratios of fruit juice water alone. PMID:10407308

  1. Synthesis of enantiopure 2-aryl-2-methoxypropionic acids and determination of their absolute configurations by X-ray crystallography.

    Science.gov (United States)

    Sekiguchi, Satoshi; Naito, Junpei; Taji, Hiromi; Kasai, Yusuke; Sugio, Akinori; Kuwahara, Shunsuke; Watanabe, Masataka; Harada, Nobuyuki

    2008-03-01

    Racemic 2-aryl-2-methoxypropionic acids were enantioresolved by the use of (S)-(-)-phenylalaninol 4. For instance, racemic 2-methoxy-2-phenylpropionic acid (+/-)-7 was condensed with phenylalaninol (S)-(-)-4 yielding a diastereomeric mixture of amides, which was easily separated by HPLC on silica gel affording the first-eluted amide (-)-13a and the second-eluted amide (+)-13b: alpha = 3.19, Rs = 3.49. The absolute configuration of amide (-)-13a was determined to be (R;S) by X-ray crystallography by reference to the S configuration of the phenylalaninol moiety. Amide (R;S)-(-)-13a was converted to oxazoline (R;S)-(-)-14a, from which enantiopure 2-methoxy-2-phenylpropionic acid (R)-(-)-7 was recovered. Other 2-aryl-2-methoxypropionic acids, (R)-(-)-8, (R)-(-)-9, (R)-(+)-10, (R)-(-)-11, and (R)-(-)-12, were similarly prepared in enantiopure forms with the use of phenylalaninol (S)-(-)-4, and their absolute configurations were clearly determined by X-ray crystallography or by chemical correlation. PMID:17559106

  2. Determination of uric acid level by polyaniline and poly (allylamine): Based biosensor.

    Science.gov (United States)

    Wathoni, Nasrul; Hasanah, Aliya Nur; Gozali, Dolih; Wahyuni, Yeni; Fauziah, Lia Layusa

    2014-01-01

    The uric acid biosensor has been much developed by immobilizing uricase enzyme into the membrane of conductive polymer and the membrane of polyelectrolyte such as polyaniline (PANI) and poly (allylamine) (PAA) respectively. The purpose of this research was to create a new amperometric uric acid biosensor by immobilization of uricase in combination between PANI and PAA membranes. The working electrode was Pt plate (0.5 mm). The auxiliary and the reference electrode were Pt wire 0.4 mm and Ag/AgCl respectively. Uricase, uric acid, PAA, pyrrole and glutaraldehyde were supplied from Sigma. All other chemical was obtained from Merck. The biosensor was created by immobilizing of uricase by a glutaraldehyde crosslinking procedure on PANI composite film on the surface of a platinum electrode while the polyelectrolyte layer of PAA were prepared via layer-by-layer assembly on the electrode, functioning as H2O2-selective film. Standard of deviation, coefficient of variation (CV) and coefficient of correlation (r) analysis were used in this study. The biosensor had a good linearity with a correlation coefficient of 0.993 and it could be used up to 27 times with the CV value of 3.97%. The presence of other compounds such as glucose and ascorbic acid gave 1.3 ± 1.13% and 3.27 ± 2.29% respectively on the interference effect toward the current response of uric acid biosensor. The polymer combination of PANI and PAA can be used as a selective matrix of uric acid biosensor. PMID:24696812

  3. Determination of uric acid level by polyaniline and poly (allylamine: Based biosensor

    Directory of Open Access Journals (Sweden)

    Nasrul Wathoni

    2014-01-01

    Full Text Available The uric acid biosensor has been much developed by immobilizing uricase enzyme into the membrane of conductive polymer and the membrane of polyelectrolyte such as polyaniline (PANI and poly (allylamine (PAA respectively. The purpose of this research was to create a new amperometric uric acid biosensor by immobilization of uricase in combination between PANI and PAA membranes. The working electrode was Pt plate (0.5 mm. The auxiliary and the reference electrode were Pt wire 0.4 mm and Ag/AgCl respectively. Uricase, uric acid, PAA, pyrrole and glutaraldehyde were supplied from Sigma. All other chemical was obtained from Merck. The biosensor was created by immobilizing of uricase by a glutaraldehyde crosslinking procedure on PANI composite film on the surface of a platinum electrode while the polyelectrolyte layer of PAA were prepared via layer-by-layer assembly on the electrode, functioning as H 2 O 2 -selective film. Standard of deviation, coefficient of variation (CV and coefficient of correlation (r analysis were used in this study. The biosensor had a good linearity with a correlation coefficient of 0.993 and it could be used up to 27 times with the CV value of 3.97%. The presence of other compounds such as glucose and ascorbic acid gave 1.3 ± 1.13% and 3.27 ± 2.29% respectively on the interference effect toward the current response of uric acid biosensor. The polymer combination of PANI and PAA can be used as a selective matrix of uric acid biosensor.

  4. PM-IRRAS Determination of Molecular Orientation of Phosphonic Acid Self-Assembled Monolayers on Indium Zinc Oxide.

    Science.gov (United States)

    Sang, Lingzi; Mudalige, Anoma; Sigdel, Ajaya K; Giordano, Anthony J; Marder, Seth R; Berry, Joseph J; Pemberton, Jeanne E

    2015-05-26

    Self-assembled monolayers (SAMs) of phosphonic acids (PAs) on transparent conductive oxide (TCO) surfaces can facilitate improvement in TCO/organic semiconductor interface properties. When ordered PA SAMs are formed on oxide substrates, interface dipole and electronic structure are affected by the functional group properties, orientation, and binding modes of the modifiers. Choosing octylphosphonic acid (OPA), F13-octylphosphonic acid (F13OPA), pentafluorophenyl phosphonic acid (F5PPA), benzyl phosphonic acid (BnPA), and pentafluorobenzyl phosphonic acid (F5BnPA) as a representative group of modifiers, we report polarization modulation-infrared reflection-absorption spectroscopy (PM-IRRAS) of binding and molecular orientation on indium-doped zinc oxide (IZO) substrates. Considerable variability in molecular orientation and binding type is observed with changes in PA functional group. OPA exhibits partially disordered alkyl chains but on average the chain axis is tilted ∼57° from the surface normal. F13OPA tilts 26° with mostly tridentate binding. The F5PPA ring is tilted 23° from the surface normal with a mixture of bidentate and tridentate binding; the BnPA ring tilts 31° from normal with a mixture of bidentate and tridentate binding, and the F5BnPA ring tilts 58° from normal with a majority of bidentate with some tridenate binding. These trends are consistent with what has been observed previously for the effects of fluorination on orientation of phosphonic acid modifiers. These results from PM-IRRAS are correlated with recent results on similar systems from near-edge X-ray absorption fine structure (NEXAFS) and density functional theory (DFT) calculations. Overall, these results indicate that both surface binding geometry and intermolecular interactions play important roles in dictating the orientation of PA modifiers on TCO surfaces. This work also establishes PM-IRRAS as a routine method for SAM orientation determination on complex oxide substrates

  5. Colorimetric and visual read-out determination of cyanuric acid exploiting the interaction between melamine and silver nanoparticles

    International Nuclear Information System (INIS)

    We present two colorimetric procedures for the determination of cyanuric acid, using silver nanoparticle-based (AgNPs) probes. The first is making use of melamine-modified AgNPs which bind to cyanuric acid through hydrogen bonding to form a large conjugate network that enhances the aggregation of AgNPs to produce an absorbance peak at 640 nm and a green coloration. In the second assay, melamine is directly added to the sample in order to form a stable complex with cyanuric acid. AgNPs are then added, resulting in the formation of an absorbance peaking at 525 nm and a color change from green (blank sample) to purple or orange-red as a function of cyanuric acid concentration. Matrix effects, that originate from the interaction of alkaline earth metals with the charged surface of the AgNPs, are mitigated through a matrix-matched calibration. In this manner, spectral transitions can be selectively attributed to the concentration of cyanuric acid, which can be even visually quantified at low mg L−1 levels with minimum sample pre-treatment and without sophisticated instrumentation. (author)

  6. [Determination of sugars, organic acids and alcohols in microbial consortium fermentation broth from cellulose using high performance liquid chromatography].

    Science.gov (United States)

    Jiang, Yan; Fan, Guifang; Du, Ran; Li, Peipei; Jiang, Li

    2015-08-01

    A high performance liquid chromatographic method was established for the determination of metabolites (sugars, organic acids and alcohols) in microbial consortium fermentation broth from cellulose. Sulfate was first added in the samples to precipitate calcium ions in microbial consortium culture medium and lower the pH of the solution to avoid the dissociation of organic acids, then the filtrates were effectively separated using high performance liquid chromatography. Cellobiose, glucose, ethanol, butanol, glycerol, acetic acid and butyric acid were quantitatively analyzed. The detection limits were in the range of 0.10-2.00 mg/L. The linear correlation coefficients were greater than 0.999 6 in the range of 0.020 to 1.000 g/L. The recoveries were in the range of 85.41%-115.60% with the relative standard deviations of 0.22% -4.62% (n = 6). This method is accurate for the quantitative analysis of the alcohols, organic acids and saccharides in microbial consortium fermentation broth from cellulose.

  7. A liquid chromatography-tandem mass spectrometry-based method for the simultaneous determination of hydroxy sterols and bile acids.

    Science.gov (United States)

    John, Clara; Werner, Philipp; Worthmann, Anna; Wegner, Katrin; Tödter, Klaus; Scheja, Ludger; Rohn, Sascha; Heeren, Joerg; Fischer, Markus

    2014-12-01

    Recently, hydroxy sterols and bile acids have gained growing interest as they are important regulators of energy homoeostasis and inflammation. The high number of different hydroxy sterols and bile acid species requires powerful analytical tools to quantify these structurally and chemically similar analytes. Here, we introduce a liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based method for rapid quantification of 34 sterols (hydroxy sterols, primary, secondary bile acids as well as their taurine and glycine conjugates). Chromatographic baseline separation of isomeric hydroxy sterols and bile acids is obtained using a rugged amide embedded C18 (polar embedded) stationary phase. The current method features a simple extraction protocol validated for blood plasma, urine, gall bladder, liver, feces, and adipose tissue avoiding solid phase extraction as well as derivatization procedures. The total extraction recovery for representative analytes ranged between 58-86% in plasma, 85% in urine, 79-92% in liver, 76-98% in adipose tissue, 93-104% in feces and 62-79% in gall bladder. The validation procedure demonstrated that the calibration curves were linear over the selected concentration ranges for 97% of the analytes, with calculated coefficients of determination (R2) of greater than 0.99. A feeding study in wild type mice with a standard chow and a cholesterol-enriched Western type diet illustrated that the protocol described here provides a powerful tool to simultaneously quantify cholesterol derivatives and bile acids in metabolically active tissues and to follow the enterohepatic circulation.

  8. Determination of uric acid level by polyaniline and poly (allylamine): Based biosensor

    OpenAIRE

    Nasrul Wathoni; Aliya Nur Hasanah; Dolih Gozali; Yeni Wahyuni; Lia Layusa Fauziah

    2014-01-01

    The uric acid biosensor has been much developed by immobilizing uricase enzyme into the membrane of conductive polymer and the membrane of polyelectrolyte such as polyaniline (PANI) and poly (allylamine) (PAA) respectively. The purpose of this research was to create a new amperometric uric acid biosensor by immobilization of uricase in combination between PANI and PAA membranes. The working electrode was Pt plate (0.5 mm). The auxiliary and the reference electrode were Pt wire 0.4 mm and Ag/A...

  9. Determination of critical conditions for the esterification of acetic acid with ethanol in the presence of carbon dioxide

    Directory of Open Access Journals (Sweden)

    G. M. Platt

    2006-09-01

    Full Text Available In this work, we present the calculation of critical coordinates for the esterification of acetic acid with ethanol in compressed carbon dioxide. Determination of the critical pressure for this system is useful, since the conversion of this reaction increases with pressure in the two-phase region, reaching a maximum at the critical point. We used a calculation framework based on a coordinate transformation for molar fractions, producing a new compositional domain. For a system with five components (acetic acid + ethanol + ethyl acetate + water + carbon dioxide and one equilibrium reaction, the compositional domain is entirely described by three independent transformed coordinates. The results obtained were compared with experimental observations presented in the literature. The results illustrate the capability of the framework used to determine critical coordinates for reactive systems, and thus its usefulness as a tool for pressure tuning for this esterification reaction in compressed carbon dioxide.

  10. Development of a rapid and simple HPLC-UV method for determination of gallic acid in Schinopsis brasiliensis

    Directory of Open Access Journals (Sweden)

    Felipe H.A. Fernandes

    2015-06-01

    Full Text Available AbstractThe aim of this work was to develop and validate an analytical method for the identification of the chemical marker of Schinopsis brasiliensis Engl., Anacardiaceae. It would determine the total polyphenols and flavonoid content by spectrophotometric methodology in the dried extract of plant. The chromatographic profiles of S. brasiliensis were determined using HPLC-UV. The liquid chromatography method was conducted on a Phenomenex Gemini NX C18 column (250 × 4.6 mm, 5 μm. The mobile phase consisted of 0.05% orthophosphoric acid: methanol. The flow rate was 1 ml/min and effluents were monitored at 271 nm. The retention time for gallic acid was 8.5 min. The described method has the advantage of being both rapid and easy. Hence it can be applied for routine quality control analysis of herbal preparation containing S. brasiliensis.

  11. Determination of protein and amino acid requirements of lactating sows using a population-based factorial approach

    DEFF Research Database (Denmark)

    Strathe, Anja Varmløse; Strathe, Anders Bjerring; Theil, P. K.;

    2015-01-01

    Determination of appropriate nutritional requirements is essential to optimize the productivity and longevity of lactating sows. The current recommendations for requirements do not consider the large variation between animals. Therefore, the aim of this study was to determine the amino acid...... for maintenance and milk. The energy balance of the sows was either negative or zero depending on feed intake being a limiting factor. Some parameters in the model were sow-specific and others were population-specific, depending on state of knowledge. Each simulation was for 1000 sows repeated 100 times using...... during lactation. The inclusion of between-sow variation gives information on safety margins when developing new dietary recommendations of amino acids and protein for lactating sows....

  12. Determination of the limit of quantification of the calorimeter using a mixture of benzoic acid and silicon dioxide

    Directory of Open Access Journals (Sweden)

    Krstić Vesna R.

    2011-01-01

    Full Text Available In recent years quality control has received a great attention in laboratory work. Implementation of the international standard ISO/IEC 17025 is necessary for any laboratory that wishes to establish quality control in its work. One of the important factors for meeting the requirements of this standard is the usage of the certified reference materials (CRM in laboratory work. In order to determine the performance of the calorimeter, benzoic acid as CRM, from AlliedSignal Riedelda Haen, Ref.: 33045 and SiO2, Pro analyze, in various mass ratios was used. The results showed that benzoic acid can be successfully utilized for the control of the entire technical and instrumental measuring range and resolve the problem of determination of the limit of detection and quantification of the calorimeter.

  13. Content determination of malic acid and lactic acid in cider by HPLC%HPLC法测定苹果酒中苹果酸及乳酸含量

    Institute of Scientific and Technical Information of China (English)

    吕兆林; 林西; 邓文红; 欧阳呓林; 张柏林

    2012-01-01

    A method to detect malic acid and lactic acid contents of cider by HPLC that containing UV detector and Symmetry C18(3.5μm×4.6mm×75mm) column was established.The column temperature was 25℃, mobile phase consisted of methanol containing 0.1%formic acid,the rate of flowing was 0.5mL/min,detection wavelength was 210nm,the injection volume was 20μL.Malic acid and lactic acid contents were detected by external standard method.The analysis results showed that correlation coefficient of the linear equation was high(it was R~2=0.9969 for malic acid and R~2=0.9999 for lactic acid).The relative standard deviation(RSD) of retention time within one day was less than 0.12%and the RSD of the peak area within one day was less than 2%, RSD of retention time in different days was below 0.12%and the RSD of the peak area in different days was below 1.82%.For malic acid,the limit of detection(LOD) was 0.43mg/L(S/N≥3),the limit of quantity(LOQ) was 1.30mg/L(S/N≥10).For lactic acid,the LOD was 1.12mg/L and the LOQ was 3.36mg/L.It was a suitable way to determine malic acid and lactic acid contents of cider with great linear relationship,favorable reproducibility and high sensitivity.%建立了HPLC测定苹果酒中苹果酸及乳酸含量的方法,即采用配紫外检测器及Symmetry C18(3.5μm×4.6mm×75mm)色谱柱的液相色谱仪,柱温25℃,流动相为含0.1%甲酸的甲醇水溶液,流速0.5mL/min,检测波长210nm,进样量20μL,通过外标法定量研究苹果酒中苹果酸及乳酸的含量。研究结果表明:该法定量线性关系良好(苹果酸标准曲线的线性相关系数R~2为0.9969,乳酸的R~2为0.9999);日内进样保留时间相对标准偏差(RSD)在0.12%以内,峰面积RSD在2%以内,日间进样保留时间的RSD在0.12%以内,峰面积的RSD在1.82%以内;苹果酸的最低检出限(LOD)(S/N≥3)可达0.43mg/L,最小检测量(LOQ)(S/N≥10)可达1.30mg/L,乳酸的LOD可达1.12mg

  14. 离子色谱法测定丁二酸合成电解液中马来酸和丁二酸%IC Determination of Maleic Acid and Succinic Acid in Electrolyte from Synthesis of Succinic Acid

    Institute of Scientific and Technical Information of China (English)

    马淳安; 邱志军; 颜飞; 赵峰鸣; 徐颖华; 褚有群

    2013-01-01

    采用离子色谱法测定丁二酸合成电解液中原料马来酸和产物丁二酸的含量.试样经Ion Pac AG19保护柱及Ion Pac AS19分析柱分离,以25 mmol·L-1氢氧化钾溶液为淋洗液,采用抑制电导器检测.马来酸和丁二酸的质量浓度在1.0~10 mg·L-1范围内与峰面积与峰高均呈线性关系.方法可用于测定合成丁二酸生产过程的不同时段溶液(起始、结束和母液)中马来酸和丁二酸的含量,有助于实现丁二酸的连续式电解合成工艺路线.%Contents of maleic acid (the raw material) and succinic acid (the products) in electrolyte from synthesis of succinic acid were determined by ion chromatography. Ion Pac AG19 protective column and Ion Pac AS19 separation column were used for separation and 25 mmol · L-1 KOH solution was used as eluant. Inhibitory conductivity detection was adopted in the determinatioa Linear relationships between values of peak area or peak height and mass concentration of maleic acid and succinic acid were kept in the range of 1. 0—10 mg · L-1. The proposed method could be used in the determination of the 2 acids in the electrolyte at different time interval (at starting and ending of electrolysis) and in the mother liquid in the synthetic process. The data obtained were helpful for the realization of synthetic technology of the continuous electrolytic production of succinic acid.

  15. Resolution of 1- and 2-naphthylmethoxyacetic acids, NMR reagents for absolute configuration determination, by use of L-phenylalaninol.

    Science.gov (United States)

    Arita, Shoko; Yabuuchi, Tetsuya; Kusumi, Takenori

    2003-08-01

    Racemic 1- and 2-naphthylmethoxyacetic acids (1NMA and 2NMA), the chiral anisotropic reagents used for absolute configuration determination of chiral secondary alcohols and primary amines, were conveniently resolved to enantiomers (>99% ee) by condensation with L-phenylalaninol (2-amino-3-phenylpropanol), chromatographic separation of the diastereomers, and hydrolysis. This method enables large-scale preparation of enantiomeric 1NMA and 2NMA. PMID:12840826

  16. Optimization of SPE/GC/HPLC Analytical Procedure for Determination of Phenol, Quinones, and Carboxylic Acids in Water Samples

    OpenAIRE

    Katarzyna Bielicka-Daszkiewicz; Monika Hadzicka; Adam Voelkel

    2012-01-01

    Chromatographic techniques are among the most useful analytical methods. Gas and liquid chromatography were used in the analysis of some organic compounds: phenol, hydroquinone, benzoquinone, and maleic and fumaric acids. The analytical way for the determination of these compounds in water samples was investigated. Solid-phase extraction (SPE) technique was used on the sample preparation step, different divinylbenzene-based sorbents were applied. Calibration curves of given compounds were lin...

  17. Comparison of high-performance ion chromatography and absorptiometric methods for the determination of phytic acid in food samples

    OpenAIRE

    Talamond, Pascale; Gallon, Georges; Guyot, Jean-Pierre; Mbome Lape, I.; Trèche, Serge

    1998-01-01

    The objective of this paper consists in defining the interest of a new high-performance ion chromatography method (HPIC) with a chemically suppressed conductivity detector for phytic acid determination in food samples. Firstly, accuracy and precision of the HPIC method were measured. Secondly, the HPIC method and a classical absorptiometric method were compared. The HPIC method was more sensitive and selective than the absorptiometric method which led to a 27% overestimation of the phytic aci...

  18. Determination of Copper-Based Fungicides by Flame Atomic Absorption Spectrometry Using Digestion Procedure with Sulfuric and Nitric Acid

    OpenAIRE

    Jelena Milinović; Rada Đurović

    2007-01-01

    Copper-based fungicides can be effectively digested by treatment with a mixture of concentrated sulfuric and nitric acid in exactly 15 minutes for the rapid determination via copper using flame atomic absorption spectrometry (AAS). Under optimum conditions, the results of copper fungicide analysis were consistent to those obtained by the AOAC’s recommended method. Recovery values ranged from 98.63 to 103.40%. Relative standard deviation values are lower than 2%. The proposed digestion procedu...

  19. Selective determination of 3,4-dihydroxyphenylacetic acid in the presence of ascorbic and uric acids using polymer film modified electrode

    Indian Academy of Sciences (India)

    Palraj Kalimuthu; S Abraham John

    2011-05-01

    We report here the highly sensitive and selective electrochemical determination of 3,4-dihydroxyphenylacetic acid (DOPAC), one of the dopamine metabolites in the presence of important interferents ascorbic acid (AA) and uric acid (UA) using an ultrathin electropolymerized film of 5-amino-1,3,4-thiadiazole-2-thiol (p-ATT) modified glassy carbon (GC) electrode in 0.20M phosphate buffer solution (pH 5.0). The bare GC electrode fails to resolve the oxidation peaks of AA, DOPAC and UA in a mixture. Further, the oxidation peak potentials of them were shifted to more positive potential with decreased peak currents in the subsequent cycles. On the other hand, the p-ATT modified electrode not only separated the voltammetric signals of AA, DOPAC and UA but also enhanced their peak currents. The amperometric current response was increased linearly with increasing DOPAC concentration in the range of 4.0 × 10−8 to 1.0 × 10−5 M and the detection limit was found to be 150pM ( =3).

  20. Spectrographic determination of lanthanides in high-purity uranium compounds, after chromatographic separation by alumina-hydrofluoric acid

    International Nuclear Information System (INIS)

    A method is presented for the determination of fourteen rare earth elements in high-purity uranium compounds by emission spectrography. The rare earths are chromatographically separated from uranium by using alumina-hydrofluoric acid. Lanthanum is used both as collector and internal standard. The technique of excitation involves a total consumption of the sample in a 17 ampere direct current arc. The range of determination is about 0.005 to 0.5 μg/g uranium. The coefficient of variation for Pr, Ho, Dy, Er, Tm, Lu, Gd and Tb amounts to 10%. (Author)