Improved sample extraction and clean-up for the GC-MS determination of BADGE and BFDGE in vegetable oil

C. Brede, I. Skjevrak, H. Herikstad, E. Anensen, R. Austvoll, T. Hemmingsen
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引用次数: 22

Abstract

A straightforward method was established for the determination of migration contaminants in olive oil with a special focus on the two can-coating migration compounds bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE). The preferred sample preparation was a single liquid-liquid extraction of compounds from the oil into 20% (v/v) methanol in acetonitrile, followed by clean-up with solid-phase extraction on aminopropyl bonded to silica. This purification procedure selectively removed all free fatty acids from the extracts without removing phenolic compounds of interest. The solid-phase extraction columns were used many times by implementing a procedure of washing out the strongly retained fatty acids with 2% acetic acid in methanol. Gas chromatography coupled with full scan (m/z 33-700) electron ionization mass spectrometry was used for the determination of several model compounds in olive oil samples. BADGE and BFDGE could be determined in the 0.05-2 mg kg−1 range in oil samples with a relative SD of <6% (six replicates). The method was used in an enforcement campaign for the Norwegian Food Control Authority to analyse vegetable oil samples from canned fish-in-oil.
改进了气相色谱-质谱法测定植物油中BADGE和BFDGE的样品提取和清理方法
建立了一种测定橄榄油中迁移性污染物的简便方法,重点研究了两种可涂覆的迁移性化合物双酚A二缩水甘油酯醚(BADGE)和双酚F二缩水甘油酯醚(BFDGE)。优选的样品制备方法是将油中的化合物单液-液萃取到20% (v/v)的乙腈甲醇中,然后用固相萃取法在与二氧化硅结合的氨基丙基上进行清理。该纯化程序选择性地从提取物中去除所有游离脂肪酸,而不去除感兴趣的酚类化合物。固相萃取柱采用2%醋酸在甲醇中洗涤强保留脂肪酸的方法进行了多次使用。采用气相色谱联用全扫描(m/z 33-700)电子电离质谱法测定了橄榄油样品中的几种模型化合物。BADGE和BFDGE可在0.05 ~ 2 mg kg - 1范围内测定,相对SD <6%(6个重复)。该方法在挪威食品管理局的一次执法行动中用于分析罐头油浸鱼的植物油样本。
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