超高效液相色谱串联质谱法测定全蛋粉中的双酚A和双酚S  

Determination of Bisphenol A and Bisphenol S in Egg Powder by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：张昊[1] 凌映茹 吉文亮[1] 刘华良[1] 朱峰[1] ZHANG Hao;LING Ying-ru;JI Wen-liang;LIU Hua-liang;ZHU Feng(Jiangsu Provincial Center for Disease Control and Prevention,Nanjing 210009,China)

机构地区：[1]江苏省疾病预防控制中心

出　　处：《食品工业科技》2019年第17期270-275,共6页Science and Technology of Food Industry

基　　金：江苏省医学重点学科(ZDXKA2016008)

摘　　要：建立超高效液相色谱-串联质谱测定全蛋粉中双酚A和双酚S的检测方法。全蛋粉经水复溶后经乙腈提取,提取液使用分散系固相萃取-基质增强脂质去除产品进行除脂,使用Oasis PRiME HLB小柱进一步净化,使用超高效液相串联质谱测定,负离子多反应监测(MRM)模式测定,内标法定量。结果显示:双酚A在1~50μg/kg范围内呈线性,相关系数为0.9991,加标回收率为98.8%~105.0%,日内和日间相对标准偏差分别为3.84%~8.58%和5.65%~8.74%,检出限为0.3μg/kg,定量限为1.0μg/kg;双酚S在0.4~20μg/kg范围内呈线性,相关系数为0.9995,加标回收率为98.5%~102.5%,日内和日间相对标准偏差分别为3.01%~7.86%和3.18%~7.03%,检出限为0.1μg/kg,定量限为0.3μg/kg。实际样品测定结果分别为:双酚A 2.4~3.8μg/kg;双酚S 0.48~0.82μg/kg。本方法前处理简单、高灵敏度适用于全蛋粉中双酚A和双酚S的日常测定。A method for the determination of BPA(bisphenol A)and BPS(bisphenol S)in egg powder with ultra-high performance liquid chromatography tandem mass spectrometry was established.The target compounds were extracted by acetonitrile from the aqueous solution of egg powder.The removal of lipid in the sample matrix was accomplished by the usage of the dSPE-EMR-Lipid(dispersive Solid-Phase Extractions Enhanced Matrix Removal Lipid),following by the further purification with an Oasis PRiMe HLB column.The contaminant was confirmed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry and the concentration was determined by internal standard method.The tandem mass spectrometry was performed in the negative electro spray ionization model and the multiple monitoring model.The results showed a good linear in the range of 1~50μg/kg for BPA with the corresponding correlation coefficient 0.9991.The recovery rate for the spiked samples ranged from 98.8%to 105.0%with relative standard deviation 3.84%~8.58%(intraday)and 5.65%~8.74%(inter-day).The limitation of detection for BPA was 0.3μg/kg and 1.0μg/kg,respectively.While results showed a good linear in the range of 0.4~20μg/kg for BPS with the corresponding correlation coefficient 0.9995.The recovery rate for the spiked samples ranged from 98.5%to 102.5%with relative standard deviation 3.01%~7.86%(intraday)and 3.18%~7.03%(inter-day).The limitation of quantitation for BPS was 0.1μg/kg and 0.3μg/kg,respectively.The concertation of compounds in actual samples was in the range of 2.4~3.8μg/kg for BPA and 0.48~0.82μg/kg for BPS respectively.The method was suitable for the daily investigation of BPA and BPS in the egg powder with the following advantages:simple sample pretreatment and high sensitivity.

关 键 词：全蛋粉 超高效液相色谱-串联质谱 分散系固相萃取-基质增强脂质去除 双酚A 双酚S 

分 类 号：TS207.3[轻工技术与工程—食品科学]