The inclusion of requirements for independent determination of arsenic, cadmium, mercury, and lead, and the current sample preparation techniques into the State Pharmacopoeia of the Russian Federation (Ph. Rus.) requires the revision of the existing limits for elemental toxicants in herbal substances and herbal medicinal products produced from them.The aim of the study was to analyse the data on elemental toxicant content obtained during quality control of herbal substances (herbs, medicinal herb mixtures, extracts, and tinctures) using current test methods and sample preparation techniques, and to compare the obtained results with the Russian and foreign scientific and specialist literature.Materials and methods: the internal data on the content of critical heavy metals and arsenic in different dosage forms of herbal medicinal products, which were obtained by inductively coupled plasma mass spectrometry after sample preparation by decomposition in closed vessels, were compared with literature data. Results: it was demonstrated that the content of lead, cadmium, and mercury in all the test samples did not exceed the Ph. Rus. limits and was consistent with the analysed literature. The arsenic content in some herbal medicinal products was higher than the established Ph. Rus. limits, but complied with the less stringent Ph. Eur. and USP requirements for herbal substances. The authors investigated the link between the content of elemental toxicants and the place of collection and the part of the plant being tested. It was shown that different types of medicinal plants had a tendency to accumulate particular elements. The authors determined the content of the elements to be controlled in extracts and tinctures. The differences in the Russian and foreign requirements for the content of elemental toxicants may be attributed to the method of obtaining experimental data that form the basis for the setting of limits.Conclusions: the results of the study confirm the validity of the existing limits for elemental toxicants in herbal medicinal products. The authors demonstrated the need to revise the existing limits for arsenic in herbal medicinal products.
Описана процедура валидации методики анализа содержания нормируемых элементных токсикантов в лекарственном растительном сырье на масс-спектрометре с индуктивно-связанной плазмой при использовании микроволновой кислотной минерализации. Предлагаемая методика пробоподготовки обеспечивает максимальный переход тяжелых металлов в раствор при неполном разложении органической матрицы с помощью концентрированной азотной кислоты. Для оценки применимости методики были выбраны образцы разных морфологических частей растений: корневища аира, трава череды, плоды можжевельника. На основании полученных экспериментальных данных была проведена оценка линейности, предела количественного определения, правильности, сходимости и внутрилабораторной прецизионности валидируемой методики. На основе определенных коэффициентов извлечения мышьяка, свинца, ртути и кадмия были рассчитаны стандартные отклонения, коэффициенты вариации, доверительные интервалы, систематические погрешности, F-критерии Фишера и t-критерии Стьюдента. Показано, что полученные статистические характеристики удовлетворяют критериям приемлемости валидационных параметров, представленным в отечественной и зарубежной нормативной документации.
Kelp can accumulate large quantities of arsenic compounds even in the absence of considerable environmental pollution. A substantial difference in toxicity between organic and inorganic arsenic compounds makes the form of arsenic relevant for the risk assessment of consuming kelp thalli and kelp-based products.The aim of the study was to develop an analytical procedure for the selective quantification of organic and inorganic arsenic in kelp thalli by inductively coupled plasma mass spectrometry and solid-phase extraction without scheduled precursors.Materials and methods. The authors studied samples of Laminaria saccharina and Laminaria japonica, spiking mixtures of chemical compounds containing arsenic in different oxidation states, and bioactive dietary supplements based on kelp thalli. Solid-phase extraction was performed using Maxi-Clean SAX cartridges. The arsenic content was determined using an Agilent 7900 inductively coupled plasma mass spectrometer.Results. Microwave-assisted extraction with deionised water ensures 91% recovery of arsenic-containing compounds from kelp thalli, and the addition of hydrogen peroxide to the extractant provides complete extraction. Solid-phase extraction with an eluent based on 3% H2O2 can extract the organic fraction from a mixture of organic and inorganic arsenic compounds without washing the inorganic fraction off the cartridge.Conclusions. The authors offer an effective analytical procedure for the selective quantification of organic and inorganic arsenic in kelp thalli and kelp-based products. This procedure allows for the isolation of arsenic-containing compounds from the organic matrix of kelp with 3% hydrogen peroxide. Solid-phase extraction with this extractant can effectively separate organic and inorganic fractions without prior neutralisation of the test solution.
Introduction. The contamination of heavy metals in medicinal plants is regional and depends on the plant’s antropogenic influence and biological properties. The purpose of the work was to study the trans-environmental transition of elemental toxicants in linden flowers by inductively coupled plasma mass spectrometry with the influence of the Moscow region anthropogenic burden. Materials and methods. One hundred eight samples were used as objects of the research, including soil, leaves and flowers of wild and cultivated linden and broadleaf trees from 36 collection sites with different levels of anthropogenic impact. The transition of elemental toxicants from soil to linden flowers was assessed directly by comparing the gross content of elements in flowers and adjacent soils. The transition of element toxicants from the atmosphere was evaluated indirectly by comparing heavy metals concentration in the linden flowers with their contents in leaves. Results. Despite the significant influence of technogenic factors on the normalized elemental toxicants in flowers of lindens, their permitted concentrations are not exceeded. To assess the trans-environment transitions, the Spearman nonparametric correlation coefficient was calculated between the content of the analyzed elements in the morphological parts of the linden and adjacent soils. It was found that the enrichment of the morphological parts of linden with aluminium, vanadium, chromium, manganese, iron, cobalt, copper, zinc, strontium, molybdenum, barium and lead occurs through the atmosphere; there is a fair correlation between the content of manganese, iron, arsenic, molybdenum and barium in the ground and morphological parts of the plant. Nickel, copper, zinc, cadmium and lead pass from the environment to the morphological parts of the linden insignificantly, mercury is practically not absorbed by the linden. Limitations. The study was conducted in Moscow and the Moscow region during one vegetative period (June 2019). Conclusions. Linden flowers are more concentrators of manganese, copper, strontium, molybdenum, barium than leaves, and they can be used as indicators of atmospheric air pollution with these elemental toxicants.
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