同位素稀释液相色谱-串联质谱法测定动物性食品中的双酚A、壬基酚及辛基酚

Determination of Bisphenol A,Nonylphenol and Octylphenol in Animal Food by Isotopic Dilution Liquid Chromatography-Tandem Mass Spectrometry

建立了动物性食品肉、蛋和奶中双酚A、壬基酚和辛基酚的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。比较了固相萃取法(SPE)和凝胶渗透色谱法(GPC)两种前处理技术,探讨了前处理过程中目标化合物背景污染的来源。最终采用乙酸乙酯-环己烷(1∶1,V/V)超声提取,经GPC净化后进行超高效液相色谱串联质谱分析。3种目标化合物的线性范围为0.25～1600!g/L,相关系数R2>0.999;对肉和鸡蛋样品,方法的定量限(LOQ)为0.2!g/kg;奶粉样品的LOQ为0.4!g/kg。目标化合物在3个不同水平的加标回收率为85.9%～117.0%,RSD<20%。应用本方法对市售动物性食品肉、蛋和奶进行了分析,壬基酚的检出率最高,含量为0.27～1357!g/kg,此外还检出了双酚A。

A comprehensive analytical method based on ultra performance liquid chromatography- tandem mass spectrometry （UPLC-MS/MS） has been developed for the simultaneous determination of bisphenol A, nonylphenol and oetylphenol in meat, egg, infant formula and milk. In this study, solid phase extraction （SPE） and gel permeation chromatography （GPC） were compared and the background contaminations of the target compounds from the pretreatment procedure were studied. Samples were extracted by ethyl acetate： cyclohexane （1：1, V/V） and purified by GPC. Satisfactory linearity （R2〉0. 999） was obtained over the range of 0.25-1600 μg/L, with limits of quantification （LOQ） of 0.2 μg/kg in meat and egg, and 0.4 μg/kg in infant formula. Mean recoveries of three target compounds （spiked at three concentration levels） ranged from 85.9 %- 117.0 %, with relative standard deviations （RSD） less than 20%. The method was applied in the analysis of meat, egg, infant formula and milk taken from Beijing. As a result, nonylphenol presented a highest detectable frequency, in the range of 0.27-1357 gg/kg. In addition, bisphenol A was also detected in this survey.