Методические подходы количественного определения бисфенолов в пищевой продукции методом ГХ–МС

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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