ОПРЕДЕЛЕНИЕ ТЯЖЕЛЫХ МЕТАЛЛОВ В МИДИИ Mytilus galloprovincialis Lamarck МЕТОДОМ ИСП-АЭС

This paper considers analytical aspects that need to be solved when studying the distribution of heavy metals in mollusks that can be used as bioindicators of the aquatic ecosystem pollution. Bivalve “Mytilus galloprovincalis Lamarc” mollusks of various age groups picked from the mussel collectors located in the Inal Bay (Black Sea) at distances of 10 and 500 m from the coastal zone were selected as the objects of the analysis. The advantages and disadvantages of the acid mineralization methods, dry ashing and microwave mineralization of the samples were considered to ensure the complete removal of all organic components of the sample, the consistency of the analytes content, and their translation into a form suitable for the subsequent spectral analysis. The operational characteristics of an ICP spectrometer (the flow rates of argon and the feed of the solution to be analyzed into a high-temperature plasma zone, the power of a high-frequency generator) as well as the influence of micro- and macro-components on the analytical signals of the elements were studied, and the conditions for the determination of heavy metals (As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, V, Sr, Zn, Mn) by the ICP-AES method in the Black Sea mussels were optimized. The distribution of heavy metals in soft and skeletal tissues of the mussels depending on their age and their habitat was examined. It was concluded that the mussels from the Black Sea accumulate Fe, Zn, Sr to a greater extent than the other metals. The distribution of metals in the mussels’ bodies of different size-age groups indicates a decrease in the concentration of most elements in their shells with an increase in the age of the organism with the exception of V, Sr, and Fe. The content of Mn, Cu decreases in the soft tissues with the increasing mollusk size, and the content of Zn, Co, Cd, As increases with the age of the animal.Keywords: bivalve mollusks, mussel Mytilus galloprovincialis Lamarc, sample preparation, determination of heavy metals, ICP-AESDOI: http://dx.doi.org/10.15826/analitika.2017.21.2.009Z.A. Temerdashev, I.I. Eletskii, A.A. Kaunova, I G. Korpakova Kuban State University, Russian Federation, 350040, Krasnodar,Stavropolskaya st., 149В работе рассмотрены аналитические аспекты, требующие решения при изучении распределения тяжелых металлов, которые могут быть использованы как биоиндикаторы загрязнения водной экосистемы, в моллюсках. В качестве объекта анализа выбраны двустворчатые моллюски мидия Mytilus galloprovincialis Lamarck различных возрастных групп, отобранные с коллекторов, расположенных в бухте Инал (Черное море), установленных на расстоянии 10 и 500 м от береговой зоны. Рассмотрены достоинства и недостатки методов сухого озоления,   традиционной кислотной минерализации и СВЧ-минерализации проб, которые должны обеспечить полное удаление всех органических компонентов образца, постоянство содержания аналитов, а также перевод их в форму, подходящую для последующего спектрального анализа. Изучены операционные характеристики спектрометра с индуктивно связанной плазмой (скорости потоков аргона и подачи анализируемого раствора в высокотемпературную зону плазмы, мощность высокочастотного генератора), а также влияние микро- и макрокомпонентов на аналитические сигналы элементов и оптимизированы условия определения тяжелых металлов (As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, V, Sr, Zn и Mn) методом АЭС-ИСП в черноморской мидии. Изучено распределение тяжелых металлов в мягких и скелетных тканях моллюсков в зависимости от их возраста и места обитания. Сделан вывод, что мидия в Черном море накапливает Fe, Zn, Sr в более значительной степени, чем другие металлы. Распределение металлов в тканях моллюсков разных размерно-возрастных групп показывает на снижение концентраций большинства элементов, за исключением V, Sr и Fe, в раковинах с увеличением возраста особи. С увеличением размеров моллюсков в мягких тканях снижается содержание Mn, Cu, а с увеличением возраста животных содержание Zn, Co, Cd, As в их тканях возрастает.Ключевые слова: двустворчатые моллюски, мидия Mytilus galloprovincialis Lamarck, пробоподготовка, определение тяжелых металлов, ИСП-АЭС  DOI: http://dx.doi.org/10.15826/analitika.2017.21.2.00

ИССЛЕДОВАНИЕ ВЗАИМОСВЯЗИ МЕЖДУ ЭЛЕМЕНТНЫМ СОСТАВОМ ВИНОГРАДА И ПОЧВОЙ РЕГИОНА ЕГО ПРОИЗРАСТАНИЯ

The influence of the grape variety and the viticultural area soils on the element content of gathered grapes was investigated, and their correlation was examined. The possible transition of metal mobile forms from the soils to the grapes was investigated based on the multi element analysis of the commercial grape samples including Cabernet Sauvignon, Riesling, Merlot and Muscat Ottonel, which were gathered from the grape fields of Krasnodar Region wineries, and soils of their cultivation. The methodical features, related to the determination of elements in the analyzed samples by ICP-AES, were discussed. The discriminant analysis was applied to the gathered data which allowed separating different viticultural areas and grape varieties with probabilities of 97 % и 94 % respectively. The canonical analysis was applied for the investigation of the correlation between the various levels in the multidimensional data. It showed the existence of the significant correlation (R = 0.95; p 0.001) between multi element contents of soil-grape systems. The relationship between the elemental contents of soil and grapes was defined, and it could be used for the determination of the production region origin for the specific grape variety.Keywords: grapes and soil, regional origin, discriminant and canonical analysis.(Russian)DOI: http://dx.doi.org/10.15826/analitika.2016.20.2.004 V.O. Titarenko1, A.A. Kaunova1, Z.A. Temerdashev1*, V. G. Popandopulo 2 1Kuban State University, ul. Stavropol’skaia., 149, Krasnodar, 350040, Russian Federation2JSC APF "Fanagoria",  ul. Mira St,49, Sennoi, Temriuk Rayon, Krasnodar Krai, 353540, Russian FederationИсследовано влияние сорта и почвы региона возделывания на элементный состав собранного винограда, рассмотрена их взаимосвязь. На основе многоэлементного анализа образцов винограда технических сортов Каберне Совиньон, Рислинг, Мерло и Мускат Оттонель, собранных с полей винодельческих предприятий Краснодарского края, а также почв, используемых для их возделывания, изучен возможный переход подвижных форм металлов из почв в виноград. Обсуждены методические особенности, связанные с определением элементов в анализируемых образцах методом ИСП-АЭС. К полученным данным применен дискриминантный анализ, позволивший с вероятностью 97 и 94 % разделить различные изучаемые участки виноградарства и сорта винограда, соответственно. Для изучения корреляции между различными данными на многомерном уровне применен канонический анализ, показавший наличие значимой корреляции (R = 0.95; p 0.001) между многоэлементными составами системы «почва – виноград». Выявлена взаимосвязь между элементным составом почв и винограда, которая может быть использована для установления региональной принадлежности продукции, полученной из конкретного сорта винограда.Ключевые слова: виноград и почвы, региональная принадлежность, дискриминантный и канонический анализ. DOI: http://dx.doi.org/10.15826/analitika.2016.20.2.00

ВИНОГРАДНЫЕ ВИНА, ПРОБЛЕМЫ ОЦЕНКИ ИХ КАЧЕСТВА И РЕГИОНАЛЬНОЙ ПРИНАДЛЕЖНОСТИ

The analysis of articles and normative documents for quality control and regional origin of wines was carried out. Chemical composition of the grapes and the wine has been considered, qualitative and quantitative changes during vinification, maturation and aging of wine were shown. The basic group of compounds contents and ratios which determine the qualitative characteristics of wines, as well as have an important role in the formation of aroma and taste of the drink was found. The prerequisites for the development of the market of counterfeit products and wine falsification methods were discussed. The analysis of scientific literature and regulatory framework governing the quality of the wines on the territory of Russia and the European Union and the existing approaches to determine their authenticity was conducted, the advantages and disadvantages are shown. The examples of using different criteria for the establishment of natural and adulterated wines have been discussed, as well as their approaches to identify and create a comprehensive system of wine production quality evaluation using methods of physicochemical analysis. The main methodological approaches to establish a wine regional origin, combining the capabilities of modern methods of analysis, mathematical modeling and statistics are analyzed, examples of their use in practice are shown.Keywords: wine, methods of analysis, quality, authenticity, regional origin, falsification, mathematical modeling (Russian)DOI: http://dx.doi.org/10.15826/analitika.2014.18.4.001 Yu.F. Yakuba1, A.A. Kaunova2, Z.A. Temerdashev2, V.O. Titarenko2, A.A. Halafjan2 1North Caucasian Regional Research Institute of Horticulture and Viticulture of the Russian Academy of Agricultural Sciences, Krasnodar, Russian Federation2 Kuban State University, Krasnodar, Russian FederationREFERENCES1. 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Method of determination of the mass concentration of the powered extract]. Moscow, Standartinform Publ., 2009. 6 p. (in Russian).68. GOST R 52391-2005. Produktsiia vinodel‘cheskaia. Metod opredeleniia massovoi kontsentratsii limonnoi kisloty [State Standard 52391-2005. Wine products. Method of determination of the mass concentration of citric acid]. Moscow, Standartinform Publ., 2007. 8 p. (in Russian).69. GOST R 51655-2000. Alkogol‘naia produktsiia i syr‘e dlia ee proizvodstva. Metod opredeleniia massovoi kontsentratsii svobodnogo i obshchego dioksida sery [State Standard 51655-2000. Alcoholic products and raw materials for its production. Method of determination of free and total sulfur dioxide]. Moscow, Standartinform Publ., 2009. 6 p. (in Russian).70. GOST R 51766-2001. Syr‘e i produkty pishchevye. Atomno-absorbtsionnyi metod opredeleniia mysh‘iaka [State Standard 51766-2001. Raw materials and food products. Determination of arsenic using Atomic absorption spectroscopy]. 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Investigation of the correlation between the elemental content of grapes and the soil of the region of its growth

Исследовано влияние сорта и почвы региона возделывания на элементный состав собранного винограда, рассмотрена их взаимосвязь. На основе многоэлементного анализа образцов винограда технических сортов Каберне Совиньон, Рислинг, Мерло и Мускат Оттонель, собранных с полей винодельческих предприятий Краснодарского края, а также почв, используемых для их возделывания, изучен возможный переход подвижных форм металлов из почв в виноград. Обсуждены методические особенности, связанные с определением элементов в анализируемых образцах методом ИСП-АЭС. К полученным данным применен дискриминантный анализ, позволивший с вероятностью 97 и 94 % разделить различные изучаемые участки виноградарства и сорта винограда, соответственно. Для изучения корреляции между различными данными на многомерном уровне применен канонический анализ, показавший наличие значимой корреляции ( R = 0.95; p < 0.001) между многоэлементными составами системы «почва - виноград». Выявлена взаимосвязь между элементным составом почв и винограда, которая может быть использована для установления региональной принадлежности продукции, полученной из конкретного сорта винограда.The influence of the grape variety and the viticultural area soils on the element content of gathered grapes was investigated, and their correlation was examined. The possible transition of metal mobile forms from the soils to the grapes was investigated based on the multi element analysis of the commercial grape samples including Cabernet Sauvignon, Riesling, Merlot and Muscat Ottonel, which were gathered from the grape fields of Krasnodar Region wineries, and soils of their cultivation. The methodical features, related to the determination of elements in the analyzed samples by ICP-AES, were discussed. The discriminant analysis was applied to the gathered data which allowed separating different viticultural areas and grape varieties with probabilities of 97 % и 94 % respectively. The canonical analysis was applied for the investigation of the correlation between the various levels in the multidimensional data. It showed the existence of the significant correlation ( R = 0.95; p < 0.001) between multi element contents of soil-grape systems. The relationship between the elemental contents of soil and grapes was defined, and it could be used for the determination of the production region origin for the specific grape variety

Determination of heavy metals in mussels Mytilus galloprovincialis Lamarc using the IСP-AES method

This paper considers analytical aspects that need to be solved when studying the distribution of heavy metals in mollusks that can be used as bioindicators of the aquatic ecosystem pollution. Bivalve Mytilus galloprovincalis Lamarck mollusks of various age groups picked from the mussel collectors located in the Inal Bay (the Black Sea) at distances of 10 and 500 m from the coastal zone were selected as the objects of the analysis. The advantages and disadvantages of the acid mineralization methods, dry ashing and microwave mineralization of the samples were considered to ensure the complete removal of all organic components of the sample, the consistency of the analytes content, and their translation into a form suitable for the subsequent spectral analysis. The operational characteristics of an ICP spectrometer (the flow rates of argon and the feed of the solution to be analyzed into a high-temperature plasma zone, the power of a high-frequency generator) as well as the influence of micro- and macro-components on the analytical signals of the elements were studied, and the conditions for the determination of heavy metals (As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, V, Sr, Zn, Mn) by the ICP-AES method in the Black Sea mussels were optimized. The distribution of heavy metals in soft and skeletal tissues of the mussels depending on their age and their habitat was examined. It was concluded that the mussels from the Black Sea accumulate Fe, Zn, Sr to a greater extent than the other metals. The distribution of metals in the mussels’ bodies of different size-age groups indicates a decrease in the concentration of most elements in their shells with an increase in the age of the organism with the exception of V, Sr, and Fe. The content of Mn, Cu decreases in the soft tissues with the increasing mollusk size, and the content of Zn, Co, Cd, As increases with the age of the animal.В работе рассмотрены аналитические аспекты, требующие решения при изучении распределения тяжелых металлов, которые могут быть использованы как биоиндикаторы загрязнения водной экосистемы, в моллюсках. В качестве объекта анализа выбраны двустворчатые моллюски мидия Mytilus galloprovincialis Lamarck различных возрастных групп, отобранные с коллекторов, расположенных в бухте Инал (Черное море), установленных на расстоянии 10 и 500 м от береговой зоны. Рассмотрены достоинства и недостатки методов сухого озоления, т радиционной кислотной минерализации и СВЧ-минерализации проб, которые должны обеспечить полное удаление всех органических компонентов образца, постоянство содержания аналитов, а также перевод их в форму, подходящую для последующего спектрального анализа. Изучены операционные характеристики спектрометра с индуктивно связанной плазмой (скорости потоков аргона и подачи анализируемого раствора в высокотемпературную зону плазмы, мощность высокочастотного генератора), а также влияние микро- и макрокомпонентов на аналитические сигналы элементов и оптимизированы условия определения тяжелых металлов (As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, V, Sr, Zn и Mn) методом АЭС-ИСП в черноморской мидии. Изучено распределение тяжелых металлов в мягких и скелетных тканях моллюсков в зависимости от их возраста и места обитания. Сделан вывод, что мидия в Черном море накапливает Fe, Zn, Sr в более значительной степени, чем другие металлы. Распределение металлов в тканях моллюсков разных размерно-возрастных групп показывает на снижение концентраций большинства элементов, за исключением V, Sr и Fe, в раковинах с увеличением возраста особи. С увеличением размеров моллюсков в мягких тканях снижается содержание Mn, Cu, а с увеличением возраста животных содержание Zn, Co, Cd, As в их тканях возрастает

Grapes cultivar assignments using the identifi ed elements-markers of grape berry and its diff erent constituent parts

Submitted 11 May 2018, received in revised form 20 September 2018Поступила в редакцию 11 мая 2018 г., после доработки 20 сентября 2018 г.The objects of our research were the samples of Cabernet and Riesling grape varieties produced in the Krasnodar Territory, Russia. The samples of grapes have been provided by their direct producers. The features of the multi-element analysis of grape berries by the method of AES-ICP were examined, their distribution in berry peel, bones and pulp as well as the revealed elements-markers of varietal belonging of grapes were studied. The conditions for preparing the samples of grapes and its main parts for the analysis by the microwave acid mineralization were optimized, ensuring a minimum level of losses of the elements to be determined. The elemental composition of Riesling and Cabernet grape varieties grown in the Kuban region was studied under the optimized conditions by the AES-ICP method. It was shown that the concentrations of some elements, both in different parts of the grapes and in different grape grades, differ significantly. The step-wise discriminant analysis, implemented in the STATISTICA program, was used to separate the samples according to the elemental “image” of the berry parts and the grape variety. The classification analysis with training allowed graphically presenting the intergroup differences between the objects. For the implementation of the discrimination process a step-by-step with exception method was selected that allowed excluding 15 elements successively, and defining the remaining 6 elements (Ba, Cr, Mg, Rb, Sr, Ti) as the markers for distinguishing the different fragments of Cabernet and Riesling grapes. A scattering diagram of canonical values was constructed that showed the localization of clusters of berries samples corresponding to the 6 groups in certain parts of the plane at a considerable distance from each other. The classification functions were developed that helped identifying the grape varieties by the content of the marker elements in one of the three parts of the grape berries - pulp, peel or bone.Объектами исследования были образцы ягод винограда сортов Каберне и Рислинг, произве­денных на территории Краснодарского края и предоставленных непосредственно их производите­лем. Рассматриваются особенности многоэлементного анализа ягод винограда методом АЭС-ИСП. Изучено распределение элементов в ягодной кожице, косточках и мякоти. Выявлены элементы-мар­керы сортовой принадлежности винограда. Оптимизированы условия подготовки проб ягод вино­града и основных ее частей к анализу способом СВЧ-кислотной минерализации, обеспечивающие минимальный уровень потерь определяемых элементов. В оптимизированных условиях методом АЭС-ИСП исследован элементный состав частей ягоды винограда сортов Рислинг и Каберне, вы­ращенных на Кубани. Показано, что концентрации некоторых элементов, как в разных частях ягод винограда, так и в различных сортах существенно различаются. Для разделения образцов по эле­ментному «образу» частей ягод и сортовой принадлежности винограда использовали пошаговый дискриминантный анализ, реализованный в программе STATISTICA. Классификационный анализ с обучением позволил графически представить межгрупповые отличия между объектами. Для осу­ществления процесса дискриминации выбран пошаговый с исключением метод, который позво­лил последовательно иск лючить 15 элементов, а оставшиеся 6 элементов (Ba, Cr, Mg, Rb, Sr и Ti) определить, как элементы-маркеры отличия различных фрагментов ягод винограда Каберне и Рислинг. Построена диаграмма рассеяния канонических значений, показывающая локализацию кластеров образцов ягод, соответствующим 6 группам в определенных частях плоскости, на зна­чительном расстоянии друг от друга. Составлены функции классификации, при помощи которых по содержанию элементов-маркеров в одной из трех частей ягоды винограда (мякоти, кожице или косточке) возможна идентификация сорта винограда.The study was supported by the Russian Foundation for Basic Research (Grant No.18-03- 00059); experiments were carried out with the use of scientific equipment of the Ecological and Analytical Center of the Kuban State University, unique identifier RFMEFI59317Х0008.Работа выполнена при финансовой поддержке Российского фонда фундаментальных исследований (проект № 18-03-00059а) с использованием научного оборудования ЦКП “Эколого-аналитический центр” Кубанского госуниверситета, уникальный идентификатор RFMEFI59317Х0008

Grape wines, problems of their quality and regional origin evaluation

Проведен анализ опубликованных работ и нормативных документов, посвященных вопросам контроля качества и региональной принадлежности вин. Рассмотрен химический состав винограда и изготавливаемой из него винодельческой продукции, показано его качественное и количественное изменение в процессе винификации, созревания и выдержки вин. Установлены основные группы соединений, содержания и соотношения которых определяют качественные характеристики вин, а также играют важную роль в формировании аромата и вкуса напитка. Обсуждены предпосылки развития рынка поддельной продукции и способы фальсификации вин. Проведен анализ научной литературы и нормативной базы, регламентирующей качество вин на территории России и стран Европейского союза, существующих подходов к определению их подлинности, указаны достоинства и недостатки. Обсуждены примеры использования различных критериев для установления натуральных и фальсифицированных вин, а также подходов их комплексной идентификации и создания системы оценки качества винодельческой продукции с помощью методов физико-химического анализа. Проанализированы основные методические подходы к установлению региональной принадлежности вин, сочетающие возможности современных методов анализа, математического моделирования и статистики, продемонстрированы примеры их использования на практике.The analysis of articles and normative documents for quality control and regional origin of wines was carried out. Chemical composition of the grapes and the wine has been considered, qualitative and quantitative changes during vinification, maturation and aging of wine were shown. The basic group of compounds contents and ratios which determine the qualitative characteristics of wines, as well as have an important role in the formation of aroma and taste of the drink was found. The prerequisites for the development of the market of counterfeit products and wine falsification methods were discussed. The analysis of scientific literature and regulatory framework governing the quality of the wines on the territory of Russia and the European Union and the existing approaches to determine their authenticity was conducted, the advantages and disadvantages are shown. The examples of using different criteria for the establishment of natural and adulterated wines have been discussed, as well as their approaches to identify and create a comprehensive system of wine production quality evaluation using methods of physicochemical analysis. The main methodological approaches to establish a wine regional origin, combining the capabilities of modern methods of analysis, mathematical modeling and statistics are analyzed, examples of their use in practice are shown