Methods and Objects of Chemical Analysis最新文献_第2页

HPLC-pharmaceutical Analysis of Lantibiotic Nisin in the Industrial Samples Including Expired Sample 包括过期样品在内的工业样品中抗生素Nisin的hplc -药学分析

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.87-91

Artur Martynov, Oksana Knysh

{"title":"HPLC-pharmaceutical Analysis of Lantibiotic Nisin in the Industrial Samples Including Expired Sample","authors":"Artur Martynov, Oksana Knysh","doi":"10.17721/moca.2023.87-91","DOIUrl":"https://doi.org/10.17721/moca.2023.87-91","url":null,"abstract":"Nisin is the most well-known representative of subtype A1 lantibiotics. This small (< 5 kDa) peptide ribosomally produced by Gram-positive bacteria belonging to Lactococcus, Streptococcus, Staphylococcus and Blautia species. Nisin exhibits antibacterial activity against a broad range of Gram-positive bacteria and may be effective against Gram-negative pathogens. For analytical semi-preparative purposes, gradient HPLC is often used in the acetonitrile concentration range from 20 to 30 % (solvent B) and a retention time of 20 to 50 min. In this study the optimal conditions for the analysis of nisin by RP-HPLC were determined: a gradient from 23 to 28 % acetonitrile (buffer B) when used as solvents: buffer A: [4 M LiClO4 – 0.1 M HClO4 ] : H2O=1:19; and buffer B: 100 % CH3CN with a retention time up to 12 min. Differences between the chromatographic profiles of expired and non-expired nisin samples have been identified. The expired nisin sample differs from the non-expired samples by the presence of asymmetric nisin A / Z peaks with significant degradation of the nisin A peak. The results of the study indicate the possibility using RP-HPLC for checking the quality and shelf life of commercial nisin samples without the need for additional purification","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135401776","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 and Validation of New Methods for Quality Control of the Antiviral Substance FAVIPIRAVIR 抗病毒药物FAVIPIRAVIR质量控制新方法的建立与验证

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.70-80

Yu.V. Scrypynets, G.O. Fedosenko, G.V. Maltsev, I.I. Chebotarska, D.I. Aleksandrova, S.N. Kashutskуy, A.V. Yegorova

引用次数: 0

Spectrophotometric and Fluorescent Determination of Hydrophobic Organic Cations in the Surfactant-modified System Mo(VI)– Bromopyrogallol Red 表面活性剂修饰体系Mo(VI) -溴吡三酚红中疏水有机阳离子的分光光度和荧光测定

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.55-62

Viktoriia Klovak, Kulichenko Sergey

{"title":"Spectrophotometric and Fluorescent Determination of Hydrophobic Organic Cations in the Surfactant-modified System Mo(VI)– Bromopyrogallol Red","authors":"Viktoriia Klovak, Kulichenko Sergey","doi":"10.17721/moca.2023.55-62","DOIUrl":"https://doi.org/10.17721/moca.2023.55-62","url":null,"abstract":"The spectrophotometric and fluorescent characteristics of the surfactant-modified molybdenum (VI) – bromopyrogallol red reagent system were studied. The hydrophobic modification was achieved by adding cationic, nonionic surfactants, or, accordingly, mixtures of surfactant modifiers into the metal reagent system. Modification of the metal reagent system with a nonionic surfactant leads to a decrease in the limit of detection of the hydrophobic organic cation in the molybdenum (VI) – bromopyrogallol red system by the fluorescence method and an increase in the contrast of the spectrophotometric reaction. The colloid-chemical state of molybdenum (VI) – bromopyrogallol red solutions in the presence of cationic surfactant, nonionic surfactant, and their mixture was also investigated. An increase in the turbidity of the investigated solutions is registered under the conditions of a decrease in the scattering factor, which, in turn, increases the limit of detection of the spectrophotometric determination of decamethoxine in the surfactant-modified molybdenum (VI) – bromopyrogallol red system. Based on the obtained results, the conditions for controlled modification of the metal reagent system with surfactants for the determination of hydrophobic organic cations by molecular spectroscopy methods were proposed. Fluorescence and spectrophotometric detection of decamethoxine content in medicines was carried out in optimized surfactant-modified molybdenum (VI) – bromopyrogallol red systems.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135401644","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

Pilot Round of Proficiency Testing Scheme for Determination of Main Quality Characteristics of Oil Cake 测定油饼主要品质特性能力测试计划试验轮

IF 0.7

Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.125-132

О.М. Chechet, О.S. Haidei, M. Ischenko, А.V. Masluk, S. Shulyak

{"title":"Pilot Round of Proficiency Testing Scheme for Determination of Main Quality Characteristics of Oil Cake","authors":"О.М. Chechet, О.S. Haidei, M. Ischenko, А.V. Masluk, S. Shulyak","doi":"10.17721/moca.2022.125-132","DOIUrl":"https://doi.org/10.17721/moca.2022.125-132","url":null,"abstract":"The new scheme of proficiency testing of laboratories for determination of main quality characteristics of oil cake was developed. In pilot round was determined such quality characteristics as moisture content (I), mass fraction of fat (II) and mass fraction of crude protein (III). The control sample was prepared from the sample of rapeseed oil cake. It was determined that control sample was sufficiently stable and homogeneous. In the round participated 22 laboratories, which used different test methods. The results were processed by the method described in ISO 13528. Based on these calculations as assigned value for characteristics I and III was chosen robust mean value and for characteristic II - mode of results. As standard deviation of proficiency testing for characteristic I was chosen robust standard deviation and for characteristics II and III was chosen value which is predicted by equation of Horwitz-Thompson. It was determined, that for characteristics I and III different test methods gives equivalent results, so some unsatisfactory results of laboratories can be attributed to laboratory bias. For characteristic II clustering of results according to measurement method in observed. It was established, that outdated standard GOST 13496.15-97 gives higher mass fraction of fat compared to other test methods.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436661","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

Patterns of the Disperse-phase Distribution of Organic Ecotoxicants in the Water of the World River Systems 世界河流水系中有机生态毒物弥散相分布模式

IF 0.7

Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.133-140

M. V. Milyukin, М.V. Gorban

引用次数: 1

Analytical Validation and Stability Indicating Studies for Simultaneous Estimation of Serdexmethylphenidate and Dexmethylphenidate by RP-HPLC in Bulk and Capsules 反相高效液相色谱法同时测定散装和胶囊中哌醋甲酯和哌醋甲酯的分析验证和稳定性研究

IF 0.7

Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.99-105

Hathibelagal Mundarinti Sudheer Kumar, Kothapalli Bannoth Chandrasekhar

{"title":"Analytical Validation and Stability Indicating Studies for Simultaneous Estimation of Serdexmethylphenidate and Dexmethylphenidate by RP-HPLC in Bulk and Capsules","authors":"Hathibelagal Mundarinti Sudheer Kumar, Kothapalli Bannoth Chandrasekhar","doi":"10.17721/moca.2022.99-105","DOIUrl":"https://doi.org/10.17721/moca.2022.99-105","url":null,"abstract":"A stability-indicating RP-HPLC method for the simultaneous determination of Serdexmethylphenidate (SER) and Dexmethylphenidate (DEX) has been developed and validated in bulk and tablet dosage forms. SER and DEX are central nervous system stimulants. This combination is used to treat attention deficit hyperactive disorder. The chromatographic analysis was carried out on a Waters C18 Column with 250mm x 4.6 and a particle size of 5 μm, using an isocratic mobile phase of Phosphate Buffer pH 4.8: Methanol (70:30, v/v) at a flow rate of 0.8 mL/min, and the eluents were monitored at an isosbestic point of 215 nm. Specificity, precision, accuracy, linearity, and robustness of the proposed method were all validated according to ICH standards. Forced degradation studies confirmed the method's stability indicating nature. SER and DEX had retention times of 2.390 and 4.602 min, respectively. The developed technique was found to be specific and accurate. SER linearity was achieved between 90-270 μg/mL, while DEX linearity was obtained between 17.50-52.50 μg/mL. SER had LOD and LOQ of 6.35 and 21.17 μg/mL, whereas DEX had LOD and LOQ of 1.18 and 3.93 μg/mL, respectively. As a result, the suggested HPLC method for the quantification of Serdexmethylphenidate (SER) and Dexmethylphenidate (DEX) was reliable, repeatable, accurate, and sensitive.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67437017","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

Contribution to the Molybdenum Blue Reaction and its Application in Soil Analysi 钼蓝反应的贡献及其在土壤分析中的应用

IF 0.7

Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.59-69

L. Angelova, N. Genova, G. Pencheva, Yasena Statkova, Violeta Yotova, A. Surleva

{"title":"Contribution to the Molybdenum Blue Reaction and its Application in Soil Analysi","authors":"L. Angelova, N. Genova, G. Pencheva, Yasena Statkova, Violeta Yotova, A. Surleva","doi":"10.17721/moca.2022.59-69","DOIUrl":"https://doi.org/10.17721/moca.2022.59-69","url":null,"abstract":"This paper presents a study on the molybdenum blue reaction (MB) as a finishing detection step in soil analysis for quantification of plant available phosphorus. An ammonium acetate/calcium lactate reagent (pH = 4.2) was used for soil phosphorus extraction. The molybdenum blue color reaction using premixed Murphy-Riley reagent and ascorbic acid as a reductant was reinvestigated. UV-Vis characteristics of MB, optimal wavelength, reaction time and concentration of reductant were studied. The effect of ascorbic acid concentration and the reaction time on linearity, bias and uncertainty was discussed. The molybdenum blue reaction was found to obey Beer’s law in the targeted concentration range of 0.04 – 1.0 mg L-1 PO43- - P. The linearity was proved by “lack-of-fit” test. The uncertainty budget was made and the uncertainty was estimated by modelling approach, as well as single laboratory and quality control approach. The recovery and the expanded uncertainty were found to be, respectively, (95.7 ± 8.7) % (P = 95 %, n = 3) and 9.2 mg PO43- - P/kg dry soil (k = 2). The results showed that the soil sample inhomogeneity and the repeatability of extraction process were the main factors which contribute to the uncertainty of measurement in soil analysis.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436788","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

A New Fluorescent Probe Based on N-(2-carboxymethyl)benzoaza-15-crown-5 for Sensitive and Selective Determination of Cu2+ 基于N-(2-羧甲基)苯并氮杂-15-冠-5的新型荧光探针对Cu2+的敏感和选择性测定

IF 0.7

Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.91-98

A. Yegorova, Yu. V. Skrypynets, I. Leonenko, D. Aleksandrova, T. Kirichenko, S. S. Basok, C. Kulygina

{"title":"A New Fluorescent Probe Based on N-(2-carboxymethyl)benzoaza-15-crown-5 for Sensitive and Selective Determination of Cu2+","authors":"A. Yegorova, Yu. V. Skrypynets, I. Leonenko, D. Aleksandrova, T. Kirichenko, S. S. Basok, C. Kulygina","doi":"10.17721/moca.2022.91-98","DOIUrl":"https://doi.org/10.17721/moca.2022.91-98","url":null,"abstract":"Copper is widely used and therefore it is a pollutant metal. It is important to develop probes that can selectively determine copper with high sensitivity. The benzoaza-15-crown-5 derivatives are used as fluorescence sensing systems and excellent spectroscopic properties are demonstrated. The “N”, “O” atoms of the heterocyclic unit act as binding sites for recognizing copper ions. A new, simple, sensitive fluorescence method for the determination of Cu2+ ions was developed and analytical characteristics of the proposed probe were estimated. The Cu2+ ions can significantly quench the fluorescence intensity of N-(2-carboxymethyl)benzoaza-15-crown-5 (Cr) in ethanol/H2O (4:6, v/v) solvent mix containing urotropine buffer (pH 7.5) at λex = 274 nm and λem = 308 nm. The probe has high photostability. Under optimal conditions, the quenching of fluorescence intensity depends on the concentration of Cu2+ ions in the range of 1.70 × 10-6 - 2.38 × 10-4 М, detection limit was 0.56 μМ. This method was applied for the determination of Cu2+ ions in drinking water. The quenching effect in the presence of copper (II) can be explained by the termination of intramolecular charge transfer from the chelate center to the aromatic part of the molecule due to chelation.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436964","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 Molecular Interferences at GDMS Analysis of Main Elements and Microalloing of High-Entropy Alloy AlCrFeCoNiCu 高熵合金AlCrFeCoNiCu主元素分析及微合金化的分子干扰研究

IF 0.7

Methods and Objects of Chemical Analysis Pub Date : 2022-01-01 DOI: 10.17721/moca.2022.43-53

V. D. Kurochkin, M. Kolomytsev, O. Romanenko

引用次数: 0

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

IF 0.7

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":null,"pages":null},"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