Methods and Objects of Chemical Analysis最新文献_第3页

Development and Validation of a Bioanalytical Method for the Quantification of Clopidogrel in Human Plasma by LC-MS/MS using the Accuracy Profiles hplc -MS/MS定量人血浆中氯吡格雷生物分析方法的建立与验证

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.153-161

Choukri El Khabbaz, A. El Orche, M. Bouatia, Amine Cheikhǁ, M. E. Faouzi, Y. Cherrah, R. Boussen, H. Bouchafra

{"title":"Development and Validation of a Bioanalytical Method for the Quantification of Clopidogrel in Human Plasma by LC-MS/MS using the Accuracy Profiles","authors":"Choukri El Khabbaz, A. El Orche, M. Bouatia, Amine Cheikhǁ, M. E. Faouzi, Y. Cherrah, R. Boussen, H. Bouchafra","doi":"10.17721/moca.2022.153-161","DOIUrl":"https://doi.org/10.17721/moca.2022.153-161","url":null,"abstract":"A basic bio-analytical method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of clopidogrel in human plasma. Clopidogrel-d3 was used as an internal standard (IS). Protein precipitation with acetonitrile for extraction of clopidogrel and it IS was used. Chromatographic separation of clopidogrel and IS was performed on a Synergi reverse phase C18 column (150 mm × 2 mm, 4 μm) using an isocratic mode. The mobile phase contained a mixture of 0.1% formic acid and acetonitrile (25 : 75) applying a flow rate of 0.4 mL/min. Ionization was performed by an electrospray ionization source (ESI), in positive MRM (Multiple Reaction Monitoring) mode. This method was validated by accuracy profiles approach using tolerance intervals limits. The calibration curve ranged from 0.0156 ng/mL to 8 ng/mL. This method can be employed effectively in bioequivalence and/or pharmacokinetics. In this method we have avoided the use of methanol in all steps of bioanalysis of clopidogrel to avert the back-conversion of clopidogrel metabolite.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436459","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Investigation of Voltammetric Behavior of Herbicide N,N’-Ethylene- 2,2’-Bipyridinium using the Copper Modified Carbon Paste Electrode 用铜修饰碳糊电极研究除草剂N,N ' -乙烯- 2,2 ' -联吡啶的伏安行为

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.28-33

M. Oubenali, Hayat El ouafy, Mouna Aamor, M. Mbarki, Aziz El Haimouti, T. EL Ouafy

{"title":"Investigation of Voltammetric Behavior of Herbicide N,N’-Ethylene- 2,2’-Bipyridinium using the Copper Modified Carbon Paste Electrode","authors":"M. Oubenali, Hayat El ouafy, Mouna Aamor, M. Mbarki, Aziz El Haimouti, T. EL Ouafy","doi":"10.17721/moca.2022.28-33","DOIUrl":"https://doi.org/10.17721/moca.2022.28-33","url":null,"abstract":"The reactivity of Diquat ion at the carbon paste electrode (C.P.E) modified by the copper (C.P.E-Cu) has been reported. The working electrode was prepared by mixing the copper with the carbon powder. The optimal potential window has been selected in the range from -1 V to 1.5 V. The effect of parameters such as pH, scan rate, preconcentration time and concentration has been studied by cyclic voltammetry. The preconcentration time is 13 minutes. The reactivity of Diquat on the electrochemical detector has been characterized by the appearance of the cathodic peak at 0.6 V in a solution of sodium sulfate (pH 3). Catalytic influence has been examined by cyclic voltammetry and electronic impedance spectroscopy. The calculated limits of detection and quantification have been 9.48·10-6 and 3.16·10-6 mol L-1, respectively. Then relative standard deviation (RSD) at 0.8·10-4 mol L-1 of Diquat was 5.77 % for nine repetitions. The analytical application was done in the determination of Diquat in real samples of apple juice with satisfying results.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436494","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Solid-phase Spectrophotometric Determination of Mo(VI) using Organopolymeric Cation Exchange Resin KU-2-8 Modified by 6,7-dihydroxy-2-phenyl-4-methylbenzopyrylium chloride 6,7-二羟基-2-苯基-4-甲基苯并氯化苄基改性有机高分子阳离子交换树脂KU-2-8固相分光光度法测定Mo(VI

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.10-16

O. Zhukovetska, E. Guzenko, A. Chebotarev, D. Snigur

引用次数: 2

Comparative Studies of Feed Samples on Salinomycin Contamination using Screening and Confirmatory Methods 盐霉素污染饲料样品的筛选与验证比较研究

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.81-90

D.V. Yanovych, Z. Zasadna, M. Rydchuk, S. Plotytsia, S.M. Kislova, O. Pazderska, S.М. Melikyan, H. Mysko

{"title":"Comparative Studies of Feed Samples on Salinomycin Contamination using Screening and Confirmatory Methods","authors":"D.V. Yanovych, Z. Zasadna, M. Rydchuk, S. Plotytsia, S.M. Kislova, O. Pazderska, S.М. Melikyan, H. Mysko","doi":"10.17721/moca.2022.81-90","DOIUrl":"https://doi.org/10.17721/moca.2022.81-90","url":null,"abstract":"The article presents the results of development of feed samples preparation method for further testing on salinomycin residues by ELISA using Salinomycin ELISA test kit, manufactured by Beijing Kwinbon Biotechnology (China) for another target matrix: tissues and eggs. Comparative study by means of different extractants and conditions of analyte extraction from feed was carried out, and recoveries’ percentages were established. Optimal conditions for two-stage extraction with methanol saline solution followed by ethyl acetate extraction from alkaline medium were experimentally selected; with further analyte concentration by evaporation and dry residue reconstitution. Application of this technique makes it possible to determine salinomycin residues in feed samples at the level of 0.35 - 0.70 mg/kg with absolute recovery of ~ 70 %. Suitability of the method was confirmed by comparative study of actually contaminated feed samples, performed by two screening methods: ELISA and TLC, and confirmatory method UHPLC-MS/MS. Developed technique has main advantages: it is simple, rapid and cost effective. Elaborated ELISA method is recommended for salinomycin residues determination at the level of cross-contamination on feed production and can be utilized in routine laboratory tests to prevent economic losses, caused by mortality of poultry and non-target animals, and to prevent salinomycine residues accumulation in food.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development of the Spectrophotometric Method for the Determination of Atorvastatin Calcium in Tablets by using Bromophenol Blue 溴酚蓝分光光度法测定片中阿托伐他汀钙含量的建立

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.111-117

N. Shulyak, S. Protsyk, T. Kuche, L. Kryskiw, O. Poliak, L. Mosula, L. Logoyda

{"title":"Development of the Spectrophotometric Method for the Determination of Atorvastatin Calcium in Tablets by using Bromophenol Blue","authors":"N. Shulyak, S. Protsyk, T. Kuche, L. Kryskiw, O. Poliak, L. Mosula, L. Logoyda","doi":"10.17721/moca.2022.111-117","DOIUrl":"https://doi.org/10.17721/moca.2022.111-117","url":null,"abstract":"A simple, rapid, and inexpensive spectrophotometric method for the determination of atorvastatin calcium in tablets has been developed. It requires only one reagent (BPB) and suitable for routine pharmaceutical analysis with less sophisticated equipment. The procedure for atorvastatin determination is based on its interaction with bromophenol blue (BPB) in medium of organic solvent. As a result of the reaction, the intensity of the band of the doubly ionized form of the BPB with a maximum at 595 nm increases. The maximum analytical signal is observed in a solution of methanol, chloroform, or acetonitrile, while ethanol and ethyl acetate turned out to be unsuitable. The optimal concentration of BPB is 4.12·10-4 M. To study the stability, the absorbance of the obtained solution was measured under optimal conditions for 45 min. The stoichiometric ratio of components in the resulting associate, determined by the method of continuous variations, is 1:1. The calibration graph is linear in the range from 4.1 to 33 μmol/L. The calculated LOD and LOQ values were 1.36 μmol/L and 4.13 μmol/L, respectively. The systematic error of the method is statistically insignificant in the whole range of calibration graph. The developed method was successfully applied for the determination of atorvastatin in tablets.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436546","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Spectrophotometric Analysis of Quaternary Drug Mixtures using Artificial Neural network model 基于人工神经网络模型的四元药物混合物分光光度分析

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.118-124

Azhar S. Hamody, F. Zankanah, S. Ali, N. Alassaf, S. B. Dikran

引用次数: 0

Chromatographic Detector Based on Adsorption-Semiconductor Sensor for Detection of Reducing Gases in Air 基于吸附-半导体传感器的空气中还原性气体检测色谱检测器

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.34-42

L. Oleksenko, N. Maksymovych, I. Matushko, G. Fedorenko, O. Ripko, L. Lutsenko

引用次数: 0

Validation of the Multiresidue Method Analysis for Pesticides in Bee Honey by UPLC-MS/MS using the Method of Samples Preparation QuEChERS 基于QuEChERS制样方法的超高效液相色谱-质谱联用分析蜜蜂蜂蜜中农药多残留方法的验证

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.141-152

Y. Omelchun, A. Kobish, N. Klochkova, L. Shevchenko

{"title":"Validation of the Multiresidue Method Analysis for Pesticides in Bee Honey by UPLC-MS/MS using the Method of Samples Preparation QuEChERS","authors":"Y. Omelchun, A. Kobish, N. Klochkova, L. Shevchenko","doi":"10.17721/moca.2022.141-152","DOIUrl":"https://doi.org/10.17721/moca.2022.141-152","url":null,"abstract":"In this paper we present the results of evaluating the suitability of the developed method for the simultaneous determination of 200 pesticide residues in bee honey using ultraperformance liquid chromatography - tandem mass spectrometry (UPLC-MS/MS). The main stages of extraction of pesticides from the matrix using QuEChERS (Quick Easy Cheap Effective Rugged Safe) sample preparation are described. Appropriate mobile phase composition was used to better identify analytes, internal standards were not applied. The studied list of pesticides is relevant for use in modern agriculture. The limit of quantification of the method (LOQ) for each of the analytes is 0.001 mg/kg, the relative standard deviation in the conditions of repeatability and reproducibility < 20.0 %, the expanded measurement uncertainty is less than the limit of regulatory requirements < 50.0 %. The calibration graph for each of the analytes had a coefficient R2 > 0.99. The use of QuEChERS sample preparation methods allows to reduce labor intensity, time and reagents, increase the accuracy and precision of research in comparison with classical methods of sample preparation. The described method makes it possible to detect a wide range of pesticides and has a fairly high sensitivity","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436364","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Modified Gran’s Plot Method for Calibrationless Potentiometric Nitrate Determination 改进的Gran图法无标定电位法测定硝酸盐

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Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.70-80

V. Doroshchuk, B. Oliinyk, S. Alekseev

引用次数: 0

An Identification and Study of Amino Acids of Erigeron annuus Herb 毛茛属植物氨基酸的鉴定与研究

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Methods and Objects of Chemical Analysis Pub Date : 2021-01-01 DOI: 10.17721/moca.2021.88-92

S. Kovalev, A. Golovach, V. Kovalev

{"title":"An Identification and Study of Amino Acids of Erigeron annuus Herb","authors":"S. Kovalev, A. Golovach, V. Kovalev","doi":"10.17721/moca.2021.88-92","DOIUrl":"https://doi.org/10.17721/moca.2021.88-92","url":null,"abstract":"Amino acids in the extract of Erigeron annuus herb were determined using an automatic precolumn derivatization with fluorenylmethyl-chloroformate and reversed-phase liquid chromatography with fluorescence and UV Vis detection. This objective is reached with automatic derivatization using o-phthalaldehyde (OPA) for primary amino acids and 9-Fluorenylmethyl chloroformate (FMOC) for secondary amino acids. Then derivatization integrates into high performance liquid chromatography (HPLC). The applied procedure is fast with easily reproduced results. The insufficient knowledge about amino acids composition of herb of Erigeron annuus is the basis for study. This work reports on content of 16 free and bound amino acids (391.41 μg/mg) in the plant raw material and influence’s evaluation of different extraction types on the amino acid profile. The total content of free amino acids was 4.66 μg/mg; proline prevailed (2.498 μg/mg). The total content of bound amino acids was 386.7 μg/mg; proline (146.8 μg/mg), arginine (67.8 μg/mg), phenylalanine (25.8 μg/mg), asparagine (24.3 μg/mg), histidine (20.4 μg/mg), alanine (18.2 μg/mg), serine (16.6 μg/mg), valine (16.0 μg/mg) were the dominant amino acids. Nine amino acids were classified as essential.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"10 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435930","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0