vedomostiregmedРегуляторные исследования и экспертиза лекарственных средствRegulatory Research and Medicine Evaluation3034-30623034-3453Federal State Budgetary Institution ‘Scientific Centre for Expert Evaluation of Medicinal Products’ of the Ministry of Health of the Russian Federation (FSBI ‘SCEEMP’)10.30895/1991-2919-2023-522vedomostiregmed-522Research ArticleРАЗРАБОТКА И ВАЛИДАЦИЯ МЕТОДИК ИССЛЕДОВАНИЯDEVELOPMENT AND VALIDATION OF ANALYTICAL PROCEDURESСелективное определение органических и неорганических форм мышьяка в слоевищах ламинарии и продуктах на их основеSelective Quantification of Organic and Inorganic Arsenic in Kelp Thalli and Kelp-Based Productshttps://orcid.org/0000-0001-9440-0950ЩукинВ. М.ShchukinV. M.

Щукин Виктор Михайлович

Петровский б-р, д. 8, стр. 2, Москва, 127051

Victor M. Shchukin

8/2 Petrovsky Blvd, Moscow 127051

schukin@expmed.ruhttps://orcid.org/0000-0001-7488-7204ЕринаА. А.ErinaA. A.

Ерина Алина Андреевна

Петровский б-р, д. 8, стр. 2, Москва, 127051

Alina A. Erina

8/2 Petrovsky Blvd, Moscow 127051

erina@expmed.ruhttps://orcid.org/0000-0002-2125-6174ШвецоваЮ. Н.ShvetsovaYu. N.

Швецова Юлия Николаевна

Петровский б-р, д. 8, стр. 2, Москва, 127051

Yulia N. Shvetsova

8/2 Petrovsky Blvd, Moscow 127051

shvetsovajn@expmed.ruhttps://orcid.org/0000-0002-1637-9081ЖигилейЕ. С.ZhigileiE. S.

Жигилей Евгения Сергеевна

Петровский б-р, д. 8, стр. 2, Москва, 127051

Evgeniya S. Zhigilei

8/2 Petrovsky Blvd, Moscow 127051

lismanes@expmed.ruhttps://orcid.org/0000-0002-9133-0835КузьминаН. Е.Kuz’minaN. E.

Кузьмина Наталия Евгеньевна - доктор химических наук.

Петровский б-р, д. 8, стр. 2, Москва, 127051

Natalia E. Kuz’mina - Dr. Sci. (Chem.).

8/2 Petrovsky Blvd, Moscow 127051

KuzminaN@expmed.ruФедеральное государственное бюджетное учреждение «Научный центр экспертизы средств медицинского применения» Министерства здравоохранения Российской ФедерацииРоссияScientific Centre for Expert Evaluation of Medicinal ProductsRussian Federation202326062023132206215Copyright © Щукин В.М., Ерина А.А., Швецова Ю.Н., Жигилей Е.С., Кузьмина Н.Е., 20232023Щукин В.М., Ерина А.А., Швецова Ю.Н., Жигилей Е.С., Кузьмина Н.Е.Shchukin V.M., Erina A.A., Shvetsova Y.N., Zhigilei E.S., Kuz’mina N.E.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.vedomostincesmp.ru/jour/article/view/522

Ламинария способна накапливать соединения мышьяка в больших количествах даже при отсутствии заметного загрязнения окружающей среды. Из-за существенных различий в токсичности органических и неорганических соединений мышьяка при оценке риска потребления слоевищ ламинарии и продуктов на их основе актуально учитывать форму его содержания.

Цель работы

Цель работы: разработка методики селективного определения содержания органических и неорганических форм мышьяка в слоевищах ламинарии без использования прекурсоров наркотических веществ на основе методов масс-спектрометрии с индуктивно-связанной плазмой (ИСП-МС) и твердофазной экстракции.

Материалы и методы

Материалы и методы: в работе были использованы образцы слоевищ Laminaria saccharina и Laminaria japonica, модельные смеси соединений мышьяка с различной степенью окисления, биологически активные добавки к пище на основе слоевищ ламинарии. Твердофазную экстракцию проводили на картриджах Maxi-Clean SAX. Содержание мышьяка определяли с помощью масс-спектрометра с индуктивно-связанной плазмой Agilent 7900.

Результаты

Результаты: установлено, что микроволновая экстракция деионизированной водой обеспечивает полноту извлечения мышьяк-содержащих соединений на уровне 91%. Добавление в экстрагент пероксида водорода приводит к полному извлечению соединений мышьяка из слоевищ ламинарии. Использование при твердофазной экстракции смеси органических и неорганических соединений мышьяка элюента на основе 3% пероксида водорода позволяет извлечь органическую фракцию, не смывая при этом с картриджа неорганические соединения мышьяка.

Выводы

Выводы: разработана методика селективного количественного определения содержания органических и неорганических форм мышьяка в слоевищах ламинарии и продуктах на их основе, позволяющая выделять мышьяк-содержащие соединения из органической матрицы ламинарии исключительно раствором 3% пероксида водорода. Использование этого экстрагента позволяет эффективно разделять органическую и неорганическую фракции на этапе твердофазной экстракции без стадии нейтрализации испытуемого раствора.

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

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

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

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.

слоевища ламинариинеорганическая форма мышьякаорганическая форма мышьякаселективное определениетвердофазная экстракциямасс-спектрометрия с индуктивно-связанной плазмойkelp thalliinorganic arsenicorganic arsenicselective quantificationsolid phase extractioninductively coupled plasma mass spectrometryРабота выполнена в рамках государственного задания ФГБУ «НЦЭСМП» Минздрава России № 056-00052-23-00 на проведение прикладных научных исследований (номер государственного учета НИР 121022400083-1)The study reported in this publication was carried out as part of publicly funded research project No. 056-00052-23-00 and was supported by the Scientific Centre for Expert Evaluation of Medicinal Products (R&D public accounting No. 121022400083-1)ReferencesПодкорытова АВ, Рощина АН. Морские бурые водоросли — перспективный источник БАВ для медицинского, фармацевтического и пищевого применения. 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The authors declare that there are no conflicts of interest present.