Pub Date : 2020-12-31DOI: 10.15826/analitika.2020.24.4.004
A. Azaryan, E. Dmitrieva, A. Temerdashev
In the last decade, the quantification of catecholamines in human biological fluids has been of great interest. Changes in catecholamine levels, such as adrenaline and dopamine, in the body lead to neurological disorders as well as several diseases, namely Alzheimer’s and Parkinson’s diseases, neuroendocrine catecholamine - producing tumors - pheochromocytoma, paraganglioma, carcinoid tumors and neuroblastoma. Moreover, different drug combinations can lead to the distortions in the human biological passport, containing the information not only about the erythropoiesis and steroid profile, but also about catecholamine levels, which are difficult to quantify in terms of sample preparation and analysis. A method has been proposed for the determination of adrenaline and dopamine dansyl derivatives in human saliva, including the derivatization and determination of analytes by ultra-high-performance liquid chromatography (UHPLC) with high resolution mass spectrometric detection. The derivatization procedure allowed obtaining less polar catecholamine derivatives, which is especially important for their quantification by reversed-phase ultra-high-performance liquid chromatography since it ensures their better retention on the sorbent. The sensitivity of these substances quantification by the proposed method was estimated; the highest sensitivity was achieved using the mobile phase consisting of the 0.1% formic acid aqueous solution and acetonitrile. The lower limit of quantification was 5 ng/mL for dansyldrenaline and 10 ng/mL for dansyldopamine respectively. The proposed technique was tested on real saliva samples obtained from volunteers to quantify catecholamine dansyl derivatives by reversed-phase high-performance liquid chromatography with high-resolution mass spectrometric detection. High sensitivity of the technique allows using it for adrenaline and dopamine determination in clinical diagnosis.
{"title":"UHPLC-HRMS determination of adrenaline and dopamine dansyl derivatives in human saliva","authors":"A. Azaryan, E. Dmitrieva, A. Temerdashev","doi":"10.15826/analitika.2020.24.4.004","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.4.004","url":null,"abstract":"In the last decade, the quantification of catecholamines in human biological fluids has been of great interest. Changes in catecholamine levels, such as adrenaline and dopamine, in the body lead to neurological disorders as well as several diseases, namely Alzheimer’s and Parkinson’s diseases, neuroendocrine catecholamine - producing tumors - pheochromocytoma, paraganglioma, carcinoid tumors and neuroblastoma. Moreover, different drug combinations can lead to the distortions in the human biological passport, containing the information not only about the erythropoiesis and steroid profile, but also about catecholamine levels, which are difficult to quantify in terms of sample preparation and analysis. A method has been proposed for the determination of adrenaline and dopamine dansyl derivatives in human saliva, including the derivatization and determination of analytes by ultra-high-performance liquid chromatography (UHPLC) with high resolution mass spectrometric detection. The derivatization procedure allowed obtaining less polar catecholamine derivatives, which is especially important for their quantification by reversed-phase ultra-high-performance liquid chromatography since it ensures their better retention on the sorbent. The sensitivity of these substances quantification by the proposed method was estimated; the highest sensitivity was achieved using the mobile phase consisting of the 0.1% formic acid aqueous solution and acetonitrile. The lower limit of quantification was 5 ng/mL for dansyldrenaline and 10 ng/mL for dansyldopamine respectively. The proposed technique was tested on real saliva samples obtained from volunteers to quantify catecholamine dansyl derivatives by reversed-phase high-performance liquid chromatography with high-resolution mass spectrometric detection. High sensitivity of the technique allows using it for adrenaline and dopamine determination in clinical diagnosis.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48139649","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}
Pub Date : 2020-12-31DOI: 10.15826/analitika.2020.24.4.001
A. Taneeva, A. Dmitrieva, V. Novikov, V. Ilyin
Current paper is devoted to the determination of phenols in surface waters using the method of gas-liquid chromatography on the nozzle chromatographic columns with different polarities of sorbents, in the capacity of which silicone elastomers, polyethylene glycol with the molecular weight of 1500, and polyoxyethylene bis arsenate obtained by arsenating polyethylene glycol-1500 were studied. It was shown that positional isomers, para - and meta – cresols, which have almost identical boiling points, were separated on polyoxyethylene bis arsenate and on the standard sorbents (SE-30 and PEG-1000) they practically do not separate and come out with a single peak. The logarithmic retention indexes were determined for the analyzed phenols and chromatographic Rorschneider polarity factors on polyoxyethylene bis arsenate, which are extremely high for ethanol (factor y) and are associated with the formation of an intermolecular hydrogen bond in the sorbate-sorbent system. It was found that polyoxyethylene bis arsenate had a linear dependence of the logarithm of the retention time on their boiling point and dipole moments. In the case of dipole moments, there was a deviation from the specified dependence for o-chlorophenol, obviously as a result of a specific substituent effect (ortho effect). Polyoxyethylene bis arsenate was used to determine phenols in the surface waters of the Kuibyshev reservoir. For this purpose, a sample preparation system based on the conversion of phenols into brominated derivatives, which have high volatility and are fairly well analyzed by gas-liquid chromatography, was used. A comparative characteristic of the limit of detection of phenols for flame ionization and thermionic detectors was given. As a result of the determination of phenols in the surface waters of the Kuibyshev reservoir, a high content of phenols was found, which fluctuates during the different seasons of the year.
{"title":"Gas chromatographic determination of phenols in surface waters using polyoxyethylene bis arsenates","authors":"A. Taneeva, A. Dmitrieva, V. Novikov, V. Ilyin","doi":"10.15826/analitika.2020.24.4.001","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.4.001","url":null,"abstract":"Current paper is devoted to the determination of phenols in surface waters using the method of gas-liquid chromatography on the nozzle chromatographic columns with different polarities of sorbents, in the capacity of which silicone elastomers, polyethylene glycol with the molecular weight of 1500, and polyoxyethylene bis arsenate obtained by arsenating polyethylene glycol-1500 were studied. It was shown that positional isomers, para - and meta – cresols, which have almost identical boiling points, were separated on polyoxyethylene bis arsenate and on the standard sorbents (SE-30 and PEG-1000) they practically do not separate and come out with a single peak. The logarithmic retention indexes were determined for the analyzed phenols and chromatographic Rorschneider polarity factors on polyoxyethylene bis arsenate, which are extremely high for ethanol (factor y) and are associated with the formation of an intermolecular hydrogen bond in the sorbate-sorbent system. It was found that polyoxyethylene bis arsenate had a linear dependence of the logarithm of the retention time on their boiling point and dipole moments. In the case of dipole moments, there was a deviation from the specified dependence for o-chlorophenol, obviously as a result of a specific substituent effect (ortho effect). Polyoxyethylene bis arsenate was used to determine phenols in the surface waters of the Kuibyshev reservoir. For this purpose, a sample preparation system based on the conversion of phenols into brominated derivatives, which have high volatility and are fairly well analyzed by gas-liquid chromatography, was used. A comparative characteristic of the limit of detection of phenols for flame ionization and thermionic detectors was given. As a result of the determination of phenols in the surface waters of the Kuibyshev reservoir, a high content of phenols was found, which fluctuates during the different seasons of the year.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47769736","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}
Pub Date : 2020-06-22DOI: 10.15826/analitika.2020.24.2.005
V. Chubarov, Elena I. Borkhonova, A. Amosova
The genesis of deposits determines wide variations in the mineral and chemical composition of iron ores. It is necessary to determine the content of not only the main ore element (Fe), but also the main rock-forming elements, especially those that affect the quality of the product obtained from the ore (for example, P and Mn). When determining Fe, Mg, Al, Si, P, Ca, Ti, and Mn in iron ores by wavelength-dispersive X-ray fluorescence analysis, two common sample preparation techniques were compared: pressing powder samples on a boric acid substrate and homogenization of calcined sample by fusion with lithium tetraborate. For each method, the repeatability of the measurement of analytical lines was evaluated, calibration equations were constructed using certified reference materials of iron ores of various types and two methods for matrix effects correction (fundamental parameters and empirical intensities) were compared. Iron ores samples from the Korshunovskoye, Rudnogorskoye and Tatyaninskoye deposits of the Angarsk ore province (north of the Irkutsk region and southeast of the Krasnoyarsk Krai) were analyzed by the certified atomic absorption and spectrophotometric techniques, and the results were compared with those obtained by X-ray fluorescence analysis. For the main ore element (Fe) and some rock-forming elements (Mg, Al, Si, P) determination, the fusion technique provided a smaller error, however, both techniques could be used to determine Ca, Ti, and Mn. The choice of the sample preparation technique for wavelength-dispersive X-ray fluorescence analysis of iron ores should be based on the appropriateness of the financial and labor costs and the necessary accuracy of the analysis. Keywords : wavelength-dispersive X-ray fluorescence analysis, iron ores, rock-forming elements, borate glasses, matrix effects correction DOI: http://dx.doi.org/10.15826/analitika.2020.24.2.005 Victor M. Chubarov 1 , Elena I. Borkhonova 2 , Alena A. Amosova 1 1 Vinogradov Institute of Geochemistry, SB RAS, 1 А Favorsky st., Irkutsk 664033, Russian Federation 2 Irkutsk State University, 1 Karl Marx st., Irkutsk 664003, Russian Federation
{"title":"Comparison of sample preparation techniques and matrix effects correction methods for X-ray fluorescence determination of total iron and rock-forming elements in iron ores","authors":"V. Chubarov, Elena I. Borkhonova, A. Amosova","doi":"10.15826/analitika.2020.24.2.005","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.2.005","url":null,"abstract":"The genesis of deposits determines wide variations in the mineral and chemical composition of iron ores. It is necessary to determine the content of not only the main ore element (Fe), but also the main rock-forming elements, especially those that affect the quality of the product obtained from the ore (for example, P and Mn). When determining Fe, Mg, Al, Si, P, Ca, Ti, and Mn in iron ores by wavelength-dispersive X-ray fluorescence analysis, two common sample preparation techniques were compared: pressing powder samples on a boric acid substrate and homogenization of calcined sample by fusion with lithium tetraborate. For each method, the repeatability of the measurement of analytical lines was evaluated, calibration equations were constructed using certified reference materials of iron ores of various types and two methods for matrix effects correction (fundamental parameters and empirical intensities) were compared. Iron ores samples from the Korshunovskoye, Rudnogorskoye and Tatyaninskoye deposits of the Angarsk ore province (north of the Irkutsk region and southeast of the Krasnoyarsk Krai) were analyzed by the certified atomic absorption and spectrophotometric techniques, and the results were compared with those obtained by X-ray fluorescence analysis. For the main ore element (Fe) and some rock-forming elements (Mg, Al, Si, P) determination, the fusion technique provided a smaller error, however, both techniques could be used to determine Ca, Ti, and Mn. The choice of the sample preparation technique for wavelength-dispersive X-ray fluorescence analysis of iron ores should be based on the appropriateness of the financial and labor costs and the necessary accuracy of the analysis. Keywords : wavelength-dispersive X-ray fluorescence analysis, iron ores, rock-forming elements, borate glasses, matrix effects correction DOI: http://dx.doi.org/10.15826/analitika.2020.24.2.005 Victor M. Chubarov 1 , Elena I. Borkhonova 2 , Alena A. Amosova 1 1 Vinogradov Institute of Geochemistry, SB RAS, 1 А Favorsky st., Irkutsk 664033, Russian Federation 2 Irkutsk State University, 1 Karl Marx st., Irkutsk 664003, Russian Federation","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-06-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46763554","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}
Pub Date : 2020-03-20DOI: 10.15826/analitika.2020.24.1.004
R. Sirotkin, V. Krylov, E. V. Elipasheva, R. E. Grubov, K. A. Lutoshkina
In order to increase the sensitivity of the ion chromatographic determination of chlorinated acetic acids ( CAAs ) in water, an emulsion microextraction preconcentration was proposed. The emulsification of extractants was performed by the ultrasonic irradiation. Diethyl and methyl tert-butyl ethers were used as extractants. The comparison of extractants showed the advantages of methyl tert-butyl ether: stable aggregation into a separate phase after the dispersion, no loss of extractant at the analysis stages due to volatility. To reduce the detection limits and improve the chromatographic separation of analytes, the organic matrix of the extract was replaced by water. It was achieved by evaporating the extractant at room temperature and dissolving the dry residue in the eluent. Also, this operation eliminated the difficulties associated with the analysis of organic extracts using the ion chromatography with conductivity detector. The absence of loss of the analytes at this stage was experimentally proven. The dependences of the efficiency of microextraction preconcentration on the various process parameters (ultrasonic exposure time, centrifugation time, volume of extractant, salt additive concentration) were established. The detection limits reached were 1∙10 -3 ‒ 8∙10 -3 mg/l, which are 20-600 times lower than the maximum permissible values for CAAs. In addition, the advantages of this preconcentration technique over the published works were the simultaneous removal of interfering impurities, small volume of water samples (4.1 ml) and chromatograph injected volume (50 μl). The relative standard deviation did not exceed 25%. The proposed method was tested by analyzing the samples of tap water. Mono- and dichloroacetic acids were detected, their content did not exceed the MAC values. Keywords : chlorinated acetic acids, ion chromatography, microextraction preconcentration DOI: http://dx.doi.org/10.15826/analitika.2020.24.1.004 R.G. Sirotkin, E.V. Elipasheva, V.A. Krylov, R.E. Grubov, K.A. Lutoshkina National Research Lobachevsky State University of Nizhny Novgorod (UNN) Gagarin pr., 23, Nizhny Novgorod, 603950, Russian Federation
{"title":"Determination of chloroacetic acids using ion chromatography with liquid-phase microextraction preconcentration","authors":"R. Sirotkin, V. Krylov, E. V. Elipasheva, R. E. Grubov, K. A. Lutoshkina","doi":"10.15826/analitika.2020.24.1.004","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.1.004","url":null,"abstract":"In order to increase the sensitivity of the ion chromatographic determination of chlorinated acetic acids ( CAAs ) in water, an emulsion microextraction preconcentration was proposed. The emulsification of extractants was performed by the ultrasonic irradiation. Diethyl and methyl tert-butyl ethers were used as extractants. The comparison of extractants showed the advantages of methyl tert-butyl ether: stable aggregation into a separate phase after the dispersion, no loss of extractant at the analysis stages due to volatility. To reduce the detection limits and improve the chromatographic separation of analytes, the organic matrix of the extract was replaced by water. It was achieved by evaporating the extractant at room temperature and dissolving the dry residue in the eluent. Also, this operation eliminated the difficulties associated with the analysis of organic extracts using the ion chromatography with conductivity detector. The absence of loss of the analytes at this stage was experimentally proven. The dependences of the efficiency of microextraction preconcentration on the various process parameters (ultrasonic exposure time, centrifugation time, volume of extractant, salt additive concentration) were established. The detection limits reached were 1∙10 -3 ‒ 8∙10 -3 mg/l, which are 20-600 times lower than the maximum permissible values for CAAs. In addition, the advantages of this preconcentration technique over the published works were the simultaneous removal of interfering impurities, small volume of water samples (4.1 ml) and chromatograph injected volume (50 μl). The relative standard deviation did not exceed 25%. The proposed method was tested by analyzing the samples of tap water. Mono- and dichloroacetic acids were detected, their content did not exceed the MAC values. Keywords : chlorinated acetic acids, ion chromatography, microextraction preconcentration DOI: http://dx.doi.org/10.15826/analitika.2020.24.1.004 R.G. Sirotkin, E.V. Elipasheva, V.A. Krylov, R.E. Grubov, K.A. Lutoshkina National Research Lobachevsky State University of Nizhny Novgorod (UNN) Gagarin pr., 23, Nizhny Novgorod, 603950, Russian Federation","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47441632","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}
Pub Date : 2020-01-01DOI: 10.15826/analitika.2020.24.1.001
T. Yankova, P. V. Melnikov, A. Alexandrovskaya, N. Zaytsev
Хемилюминесцентный метод определения микроорганизмов, основанный на определении аденозинтрифосфата (АТФ), который содержится в клетках бактерий, в целом состоит из трех стадий: пробоподготовки, устраняющей мешающее влияние матрицы образца, аналитической реакции и обработки полученного сигнала. Данная работа направлена на совершенствование второго этапа анализа – оптимизацию условий проведения хемилюминесцентной реакции. АТФ инициирует хемилюминесценцию люминола, интенсивность которой прямо пропорциональна концентрации АТФ. Нами были оптимизированы условия проведения данной хемилюминесцентной реакции для определения общего микробного числа (ОМЧ) в водных средах. Для этого проведено сравнение двух хемилюминесцентных реагентов: люминола и его гидрофобного аналога N-октиллюминола, который способен образовывать мицеллы. Переход к хемилюминесцентной системе на основе N-октиллюминола позволил увеличить чувствительность метода в 5.5 раз за счет микроконцентрирования аналита в ядре собственных мицелл. Нами было определено и обсуждено влияние неионогенных поверхностно-активных веществ на хемилюминесцентный способ определения бактерий. При этом выявлено, что добавление неионогенных поверхностно-активных веществ ухудшает аналитический сигнал за счет уменьшения локальной концентрации АТФ в мицеллах. Для аналитических систем, основанных на окислении люминола и N-октиллюминола, определены показатели точности, правильности, повторяемости и внутрилабораторной прецизионности. Применение разработанной хемилюминесцентной системы позволило существенно улучшить методику определения ОМЧ с переходом от качественного определения микроорганизмов к количественному измерению в диапазоне от 4×105 до 1×107 КОЕ/мл. При этом погрешность определения была снижена с 80 до 26 %. Ключевые слова: хемилюминесценция, мицеллярные системы, люминол, аналог люминола, общее микробное число, поверхностно-активные вещества
{"title":"Improvements of laboratory methods for determining the microbial count using chemiluminescent reactions in organized molecular systems","authors":"T. Yankova, P. V. Melnikov, A. Alexandrovskaya, N. Zaytsev","doi":"10.15826/analitika.2020.24.1.001","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.1.001","url":null,"abstract":"Хемилюминесцентный метод определения микроорганизмов, основанный на определении аденозинтрифосфата (АТФ), который содержится в клетках бактерий, в целом состоит из трех стадий: пробоподготовки, устраняющей мешающее влияние матрицы образца, аналитической реакции и обработки полученного сигнала. Данная работа направлена на совершенствование второго этапа анализа – оптимизацию условий проведения хемилюминесцентной реакции. АТФ инициирует хемилюминесценцию люминола, интенсивность которой прямо пропорциональна концентрации АТФ. Нами были оптимизированы условия проведения данной хемилюминесцентной реакции для определения общего микробного числа (ОМЧ) в водных средах. Для этого проведено сравнение двух хемилюминесцентных реагентов: люминола и его гидрофобного аналога N-октиллюминола, который способен образовывать мицеллы. Переход к хемилюминесцентной системе на основе N-октиллюминола позволил увеличить чувствительность метода в 5.5 раз за счет микроконцентрирования аналита в ядре собственных мицелл. Нами было определено и обсуждено влияние неионогенных поверхностно-активных веществ на хемилюминесцентный способ определения бактерий. При этом выявлено, что добавление неионогенных поверхностно-активных веществ ухудшает аналитический сигнал за счет уменьшения локальной концентрации АТФ в мицеллах. Для аналитических систем, основанных на окислении люминола и N-октиллюминола, определены показатели точности, правильности, повторяемости и внутрилабораторной прецизионности. Применение разработанной хемилюминесцентной системы позволило существенно улучшить методику определения ОМЧ с переходом от качественного определения микроорганизмов к количественному измерению в диапазоне от 4×105 до 1×107 КОЕ/мл. При этом погрешность определения была снижена с 80 до 26 %. Ключевые слова: хемилюминесценция, мицеллярные системы, люминол, аналог люминола, общее микробное число, поверхностно-активные вещества","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"76 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252447","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}
Pub Date : 2020-01-01DOI: 10.15826/analitika.2020.24.3.004
Y. M. Pliashak, S. Leschev, A. I. Palianskikh, L. Belysheva, M. Zayats
of food synthetic acid dyes (E 102, E 104, E 110, E 122, E 123, E 124, E 127, E 128, E 129, E 131, E 132, E 133, E 142, E 143, E 151, E 155) from the aqueous solutions with organic solvents and solutions of trioctyl methylammonium chloride (TOMAC) was studied. The determination of the dyes content in the phases was performed by photometry, the estimated parameters were the distribution coefficient ( D ) and the degree of extraction ( R , %). The principle possibility of selective extraction by organic solvents (chloroform, isoamyl alcohol) of the E 127 dye ( D > 24, R > 96 %), prohibited for use by the Technical Regulations of the Customs Union 029/2012, was shown. To a lesser extent, E 104 ( D = 1, R = 50 %) was extracted with isoamyl alcohol. Chloroform and toluene solutions of TOMAC with the concentration of 1·10 -2 M quantitatively extract the studied SD from the aqueous solutions with the concentration of 2·10 -4 M, but chloroform was the most effective. Based on the obtained data, the method for the quantitative determination of SD in liquid food products (juices, beverages, wines, etc.) was proposed. It consisted of the preliminary E 127 removal with chloroform and colored hydrophobic impurities, subsequent E 104 removal with isoamyl alcohol followed by the extraction of the remaining SD using the chloroform solution of TOMAC, and photometry of the extract. The conducted studies were confirmed by HPLC – DAD method.
{"title":"Extraction-photometric determination of synthetic food dyes in liquid food products","authors":"Y. M. Pliashak, S. Leschev, A. I. Palianskikh, L. Belysheva, M. Zayats","doi":"10.15826/analitika.2020.24.3.004","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.3.004","url":null,"abstract":"of food synthetic acid dyes (E 102, E 104, E 110, E 122, E 123, E 124, E 127, E 128, E 129, E 131, E 132, E 133, E 142, E 143, E 151, E 155) from the aqueous solutions with organic solvents and solutions of trioctyl methylammonium chloride (TOMAC) was studied. The determination of the dyes content in the phases was performed by photometry, the estimated parameters were the distribution coefficient ( D ) and the degree of extraction ( R , %). The principle possibility of selective extraction by organic solvents (chloroform, isoamyl alcohol) of the E 127 dye ( D > 24, R > 96 %), prohibited for use by the Technical Regulations of the Customs Union 029/2012, was shown. To a lesser extent, E 104 ( D = 1, R = 50 %) was extracted with isoamyl alcohol. Chloroform and toluene solutions of TOMAC with the concentration of 1·10 -2 M quantitatively extract the studied SD from the aqueous solutions with the concentration of 2·10 -4 M, but chloroform was the most effective. Based on the obtained data, the method for the quantitative determination of SD in liquid food products (juices, beverages, wines, etc.) was proposed. It consisted of the preliminary E 127 removal with chloroform and colored hydrophobic impurities, subsequent E 104 removal with isoamyl alcohol followed by the extraction of the remaining SD using the chloroform solution of TOMAC, and photometry of the extract. The conducted studies were confirmed by HPLC – DAD method.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"231 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252935","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}
Pub Date : 2020-01-01DOI: 10.15826/analitika.2020.24.2.007
V. M. Ostrovskaya, E. A. Reshetnyak, O. Chernyshova, E. Bryleva
RIP-Pd-Test reagent indicator paper based on 1-phenyl-5-(3,4-dihydro-6-methyl-4-oxo-3H-pyrimidin-2-yl)-formazan-6-cellulose has been proposed for determining the palladium content using the sorption-reflectometry and visual-test methods in objects of complex composition. The RIP synthesis technique was described. The estimated composition of the metal complex formed as a result of the heterogeneous indicator reaction at pH 1.5–2.5 was indicated, and the forced coordination of palladium : reagent = 1:1 was ensured. When the RIP interacted with palladium (II) ions, the yellow indicator strip became green with different intensities. Under the selected conditions, the high selectivity for the detection and determination of Pd(II) was shown. With the help of the «Ecotest-2040» portable reflectometer, the reflectometry measurements were carried out using the red LED with the radiation wavelength of 660 nm. For the visual testing, the color scales were used. The indicator reaction was proposed to be carried out in three modes: without concentration and with concentration of the test solution in 100 and 1000 times on the reaction indicator zone of the paper strip (using the pocket pumping device). By the statistical method, the limit of Pd(II) determination for the visual test method (40, 0.47, 0.042 mg/l) was estimated. The palladium detection limit using the reflectometer (19, 0.22, 0.018 mg/l) for the three modes, respectively, was calculated by 3s criterion. The found values of the limiting concentrations were comparable with the metrological characteristics of the known analysis methods in which solid-phase reagents were used. The trueness of the palladium determinations in technological objects of complex composition and drugs has been proven by the independent methods - atomic emission, spectrophotometric and gravimetric methods of analysis. The value of the relative standard deviation of the determined Pd(II) concentration using the portable reflectometer did not exceed 7%.
{"title":"Reflectometric and visual test determination of Pd(II) in objects of complex composition using the indicator paper","authors":"V. M. Ostrovskaya, E. A. Reshetnyak, O. Chernyshova, E. Bryleva","doi":"10.15826/analitika.2020.24.2.007","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.2.007","url":null,"abstract":"RIP-Pd-Test reagent indicator paper based on 1-phenyl-5-(3,4-dihydro-6-methyl-4-oxo-3H-pyrimidin-2-yl)-formazan-6-cellulose has been proposed for determining the palladium content using the sorption-reflectometry and visual-test methods in objects of complex composition. The RIP synthesis technique was described. The estimated composition of the metal complex formed as a result of the heterogeneous indicator reaction at pH 1.5–2.5 was indicated, and the forced coordination of palladium : reagent = 1:1 was ensured. When the RIP interacted with palladium (II) ions, the yellow indicator strip became green with different intensities. Under the selected conditions, the high selectivity for the detection and determination of Pd(II) was shown. With the help of the «Ecotest-2040» portable reflectometer, the reflectometry measurements were carried out using the red LED with the radiation wavelength of 660 nm. For the visual testing, the color scales were used. The indicator reaction was proposed to be carried out in three modes: without concentration and with concentration of the test solution in 100 and 1000 times on the reaction indicator zone of the paper strip (using the pocket pumping device). By the statistical method, the limit of Pd(II) determination for the visual test method (40, 0.47, 0.042 mg/l) was estimated. The palladium detection limit using the reflectometer (19, 0.22, 0.018 mg/l) for the three modes, respectively, was calculated by 3s criterion. The found values of the limiting concentrations were comparable with the metrological characteristics of the known analysis methods in which solid-phase reagents were used. The trueness of the palladium determinations in technological objects of complex composition and drugs has been proven by the independent methods - atomic emission, spectrophotometric and gravimetric methods of analysis. The value of the relative standard deviation of the determined Pd(II) concentration using the portable reflectometer did not exceed 7%.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252529","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}
Pub Date : 2020-01-01DOI: 10.15826/analitika.2020.24.2.004
I. Zenkevich, A. I. Desyatova
The previously proposed approach for controlling the inertness of gas chroma to graphic (GC) systems was based on the determination of peak area ratios for polar and non-polar constituents of test-solutions ( S rel = S polar / S non-polar ) for the series of samples obtained by the consequent dilutions (for the 10-times dilutions the number of samp les was five). This appro ach was modified with the purpose of increasing the relia bi lity of evaluating the minimal quantities of analytes ( m lim ), for which one can neglect the insufficient inertness of GC systems. In addition to that, the simplification of experimental opera tions and minimizing the number of parallel determina ti ons as well as more rational algorithm of data processing was achieved. The essence of the modified appro ach was the approximation of S rel = f (p m ) data sets with the 3 rd degree polynomials, following by comparing these data with the averaged S rel (with standard deviations) values for the most reproducible S rel values of three test-so lu tions with the highest concentrations of test-compounds. It was shown that the limits of the inertness for the WCOT-column (with the standard non-polar polydimethylsiloxane stationary phase) were from the fractions of nano gram to several nanograms of polar analytes in the chromatographic zone. The results for the test-samples contained some polar constituents (e.g., benzyl alco hol) which lead to suggesting that the integral manifestations of the insufficient inertness could be caused not only by the influence of chromatographic systems, but also by the sorp tion of polar analytes on the surfaces of vials used for the dilution of test-samples. The differences in m lim values for the same polar components at the same analytical conditions, when the dilutions were carried out in the glass or polypropylene vials, were revealed.
{"title":"Modification of inertness test for gas chromatographic systems","authors":"I. Zenkevich, A. I. Desyatova","doi":"10.15826/analitika.2020.24.2.004","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.2.004","url":null,"abstract":"The previously proposed approach for controlling the inertness of gas chroma to graphic (GC) systems was based on the determination of peak area ratios for polar and non-polar constituents of test-solutions ( S rel = S polar / S non-polar ) for the series of samples obtained by the consequent dilutions (for the 10-times dilutions the number of samp les was five). This appro ach was modified with the purpose of increasing the relia bi lity of evaluating the minimal quantities of analytes ( m lim ), for which one can neglect the insufficient inertness of GC systems. In addition to that, the simplification of experimental opera tions and minimizing the number of parallel determina ti ons as well as more rational algorithm of data processing was achieved. The essence of the modified appro ach was the approximation of S rel = f (p m ) data sets with the 3 rd degree polynomials, following by comparing these data with the averaged S rel (with standard deviations) values for the most reproducible S rel values of three test-so lu tions with the highest concentrations of test-compounds. It was shown that the limits of the inertness for the WCOT-column (with the standard non-polar polydimethylsiloxane stationary phase) were from the fractions of nano gram to several nanograms of polar analytes in the chromatographic zone. The results for the test-samples contained some polar constituents (e.g., benzyl alco hol) which lead to suggesting that the integral manifestations of the insufficient inertness could be caused not only by the influence of chromatographic systems, but also by the sorp tion of polar analytes on the surfaces of vials used for the dilution of test-samples. The differences in m lim values for the same polar components at the same analytical conditions, when the dilutions were carried out in the glass or polypropylene vials, were revealed.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252761","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}
Pub Date : 2020-01-01DOI: 10.15826/analitika.2020.24.2.003
O. Rudakov, O. V. Chernousova, R. G. Cherepakhina, Ya.O. Rudakov
{"title":"Сolorimetric determination of admixtures in cements by mobile devices","authors":"O. Rudakov, O. V. Chernousova, R. G. Cherepakhina, Ya.O. Rudakov","doi":"10.15826/analitika.2020.24.2.003","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.2.003","url":null,"abstract":"","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252221","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}
Pub Date : 2020-01-01DOI: 10.15826/analitika.2020.24.2.001
A. Titova, V. Postnov, S. Savinov, N. V. Stolyarova, N. Ivanenko, V. Chuchina, A. Gubal, A. Ganeev
The pollution of the environment with uranium dictates the need to control the concentration of this element in natural waters to the permissible limits for the stability of the ecosystems and public health. In 2011, WHO set maximum permissible concentration of uranium in water to 0.03 ppm due to the strong toxicity and radioactivity of uranium in water. Therefore, the continuous monitoring of uranium content is an important task for the safety and health of the citizens. To determine the low uranium content in natural waters, the conservation of the studied solutions is necessary. However, this method of storage and transportation is not always simple. In the current paper, as a convenient method of concentrating uranium, preserving the sample and transporting it, we used the method of sorbing uranium on sorbents. Single-layer carbon nanotubes were used as sorbents. Their surfaces were modified using wet chemical oxidation and synthesis with Aerosil A-380 silica. Two schemes were considered for concentrating the uranium on the surface of the sorbent: individual carbon nanotubes and nanotubes modified with silica. The direct analysis was used to determine the content of uranium in the sorbent, namely, time-of-flight mass spectrometry with the pulsed glow discharge (GD-MS). The most effective approach for the determination of uranium in water was the sorption of uranium on the tablet consisting of oxidized nanotubes modified with silica. The limit of detection in this case was 0.2 ppb.
{"title":"Determination of uranium in aqueous solutions by the time-of-flight mass-spectrometry with a pulsed glow discharge after its accumulation on the oxidized carbon nanotubes","authors":"A. Titova, V. Postnov, S. Savinov, N. V. Stolyarova, N. Ivanenko, V. Chuchina, A. Gubal, A. Ganeev","doi":"10.15826/analitika.2020.24.2.001","DOIUrl":"https://doi.org/10.15826/analitika.2020.24.2.001","url":null,"abstract":"The pollution of the environment with uranium dictates the need to control the concentration of this element in natural waters to the permissible limits for the stability of the ecosystems and public health. In 2011, WHO set maximum permissible concentration of uranium in water to 0.03 ppm due to the strong toxicity and radioactivity of uranium in water. Therefore, the continuous monitoring of uranium content is an important task for the safety and health of the citizens. To determine the low uranium content in natural waters, the conservation of the studied solutions is necessary. However, this method of storage and transportation is not always simple. In the current paper, as a convenient method of concentrating uranium, preserving the sample and transporting it, we used the method of sorbing uranium on sorbents. Single-layer carbon nanotubes were used as sorbents. Their surfaces were modified using wet chemical oxidation and synthesis with Aerosil A-380 silica. Two schemes were considered for concentrating the uranium on the surface of the sorbent: individual carbon nanotubes and nanotubes modified with silica. The direct analysis was used to determine the content of uranium in the sorbent, namely, time-of-flight mass spectrometry with the pulsed glow discharge (GD-MS). The most effective approach for the determination of uranium in water was the sorption of uranium on the tablet consisting of oxidized nanotubes modified with silica. The limit of detection in this case was 0.2 ppb.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252394","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}
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