固相萃取-高效液相色谱串联质谱法测定植物油中6种酚类环境激素

摘要

A simple and quick analysis method was established for the determination of six phenol environmental hormones (bisphenol A,bisphenol B,bisphenol F,4-nonylphwnol,4-n-nonylphenol,octylphenol) in plant oil by HPLC-MS/MS and solid phase extraction (SPE).After addition of the isotope internal standard,the samples were dispersed with hexane and cleaned by Carb/NH2 solid phase extraction column,and then analyzed by HPLC-MS/MS in the multiple reaction monitoring (MRM) mode.Under the optimal experimental conditions,the calibration curves of six phenol environmental hormones were linear in the range of 0.40-50.0 μg/L with correlation coefficients more than 0.994.The limits of detection and the limits of qualification of the method were 0.4-0.8 μg/kg and 1.2-2.4 μg/kg,respectively.The mean recovery rate of six phenol environmental hormones were 87.9％-98.0％ combining with the relative standard deviation ranging from 4.37％-11.00％.The method was suitable for the identification and quantification of six phenol environmental hormones in plant oil due to its simplicity and accuracy.%建立了一种简单、快速测定植物油中6种酚类环境激素(双酚A、双酚B、双酚F、4-壬基酚、4-n-壬基酚、辛基酚)的固相萃取净化-液相色谱串联质谱的分析方法.样品加入同位素内标后,经正己烷溶解,Carb/NH2固相萃取柱净化,高效液相色谱分离,串联四极杆电喷雾离子源负模式及多反应监测模式检测.双酚A等6种环境激素在0.40～200 μg/L范围内线性关系良好,相关系数均＞0.994;方法的检出限为0.4～0.8 μg/kg,定量限为1.2～2.4 μg/kg;平均回收率为87.9％～98.0％,相对标准偏差为4.37％～11.00％.该方法具有净化效果好、定量准确、灵敏快速的特点,适用于植物油中双酚A等6种环境激素的定量分析检测.