foodsystFood systemsПищевые системы2618-97712618-7272Федеральный научный центр пищевых систем им. В.М. Горбатова РАН10.21323/2618-9771-2026-9-1-119-128foodsyst-1006Research ArticleСтатьиMethodological approaches to quantification of bisphenols in foods by GC–MSМетодические подходы количественного определения бисфенолов в пищевой продукции методом ГХ–МСhttps://orcid.org/0000-0001-7693-3032УтьяновД. А.UtyanovD. A.

Утьянов Дмитрий Александрович — кандидат технических наук, научный сотрудник, лаборатория «Научно-методические работы, биологические и аналитические исследования»

109316, Москва, ул. Талалихина, 26

Dmitry A. Utyanov, Scientific Worker, Laboratory of Scientifically-Methodical Works and Control-Analytical Researches

26, Talalikhin str., 109316, Moscow

d.utyanov@fncps.ruhttps://orcid.org/0000-0002-9395-705XВостриковаН. Л.VostrikovaN. L.

Вострикова Наталья Леонидовна — доктор технических наук, Руководитель Научно-исследовательского испытательного центра

109316, Москва, ул. Талалихина, 26

Natalia L. Vostrikova, Doctor of Technical Sciences, Head of the Research Testing Center

26, Talalikhin str., 109316, Moscow

n.vostrikova@fncps.ruhttps://orcid.org/0000-0002-4492-7639ГутновА. В.GutnovA. V.

Андрей В. Гутнов — кандидат химических наук, доцент, кафедра химии и биотехнологии

362025, Республика Северная Осетия — Алания, Владикавказ, Ватутина, 44–46

Andrey V. Gutnov, Candidate of Chemical Sciences, Docent, Department of Chemistry and Biotechnology

44–46, Vatutina str., Vladikavkaz, North Ossetia — Alania, 362025

gutnov@mail.ruhttps://orcid.org/0000-0003-1862-7410ЗахароваВ. А.ZakharovaV. A.

Захарова Варвара Алексеевна — младший научный сотрудник, лаборатория «Научно-методические работы, биологические и аналитические исследования»

109316, Москва, ул. Талалихина, 26

Varvara A. Zakharova, Junior Researcher, Laboratory of Scientifically- Methodical Works and Control-Analytical Researches

26, Talalikhin str., 109316, Moscow

v.zakharova@fncps.ruhttps://orcid.org/0009-0003-7660-1291ИвановА. А.IvanovA. A.

Иванов Алексей Антонович — старший техник, лаборатория «Научно-методические работы, биологические и аналитические исследования»

109316, Москва, ул. Талалихина, 26

Aleksei A. Ivanov, Senior Technician, Laboratory of Scientifically-Methodical Works and Control-Analytical Researches

26, Talalikhin str., 109316, Moscow

a.ivanov@fncps.ruhttps://orcid.org/0000-0003-2719-9649ПолищукЕ. К.PolishchukE. K.

Полищук Екатерина Константиновна — младший научный сотрудник, Экспериментальная клиника-лаборатория биологически активных веществ животного происхождения

109316, Москва, ул. Талалихина, 26

Ekaterina K. Polishchuk, Junior Researcher, Experimental Clinic — Research Laboratory of Biologically Active Substances of an Animal Origin

26, Talalikhin str., 109316, Moscow

e.politchuk@fncps.ruФедеральный научный центр пищевых систем им. В. М. ГорбатоваРоссияV. M. Gorbatov Federal Research Center for Food SystemsRussian FederationОсетинский государственный университетРоссияNorth-Ossetian State UniversityRussian Federation20261704202691119128Copyright © Utyanov D.A., Vostrikova N.L., Gutnov A.V., Zakharova V.A., Ivanov A.A., Polishchuk E.K., 20262026Утьянов Д.А., Вострикова Н.Л., Гутнов А.В., Захарова В.А., Иванов А.А., Полищук Е.К.Utyanov D.A., Vostrikova N.L., Gutnov A.V., Zakharova V.A., Ivanov A.A., Polishchuk E.K.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.fsjour.com/jour/article/view/1006

The paper presents the developed and validated method for quantification of six out of seven selected bisphenols in foods by gas chromatography with mass spectrometric detection after silylation derivatization. Sample preparation is based on extraction of analytes using QuEChERS with the following purification of extracts using SPE and concentration before chromatographic analysis. The procedure of sample preparation includes defatting using hexane and dispersive solid phase purification. Derivatization is carried out with the use of MSTFA under controlled temperature to obtain stable volatile derivatives suitable for GC–MS analysis. The quantitative characteristics of the method were obtained that included limits of detection (LOD) and limits of quantification (LOQ) for each of the studied bisphenols. For each analyte, a degree of extraction at three levels of introduction was calculated, being no less than 88%, which corroborates reproducibility and sufficient performance of the chosen scheme of sample preparation. Chromatographic conditions ensure separation of the studied bisphenols, except one critical pair, and stability of retained signals during serial analysis. For all compounds, characteristic mass spectra were obtained and ion transitions used for identification were determined. The presented method is suitable to a larger extent in research on studying factors that increase a degree of migration of bisphenols into foods. The paper presents all necessary stages for analysis of food products: detailed description of the process of sample preparation, protocol of derivatization, equipment for the GC–MS system. The process of sample preparation is designed for complex food matrices that require a high degree of purification for the following analysis.

В работе разработана и валидирована методика количественного определения шести из семи выбранных бисфенолов в пищевой продукции методом газовой хроматографии с масс-спектрометрическим детектированием после силилирующей дериватизации. Пробоподготовка основана на экстракции аналитов с использованием QuEChERS и последующей очисткой экстрактов ТФЭ и концентрированием перед хроматографическим анализом. Процедура пробоподготовки включает гексановое обезжиривание и дисперсную твердофазную очистку. Дериватизация выполняется с использованием МСТФА при контролируемой температуре для получения стабильных летучих производных, пригодных для ГХ–МС анализа. Получены количественные характеристики метода, включающие пределы обнаружения (LOD) и пределы количественного определения (LOQ) для каждого из исследуемых бисфенолов. Для каждого аналита рассчитана степень экстракции при трёх уровнях внесения, которая составляет не менее 88%, что подтверждает воспроизводимость и достаточную эффективность выбранной схемы подготовки пробы. Хроматографические условия обеспечивают разделение исследуемых бисфенолов, кроме одной критической пары, и устойчивость удерживаемых сигналов в ходе серийного анализа. Для всех соединений получены характерные масс-спектры и определены ионные переходы, используемые для идентификации. Представленная методика подойдет в большей степени исследовательских работ по изучению факторов, увеличивающих степень миграции бисфенолов в пищевые продукты. В статье приведены все необходимые этапы для исследования пищевой продукции: детальное описание процесса подготовки пробы, протокол дериватизации, инструментальные установки для ГХ–МС системы. Процесс подготовки пробы сделан для сложных пищевых матриц, которые требуют высокой степени очистки для последующего анализа.

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The authors declare that there are no conflicts of interest present.