摘要
建立了QuEChERS/GC-MS法测定鱼、虾中雌二醇（ES）和己烯雌酚（DES）残留的分析方法。样品中依次加入无水硫酸镁和乙酸乙酯后均质提取,提取液以中性氧化铝分散剂净化,氮气吹干,经双（三甲基硅烷基）三氟乙酰胺（BSTFA）与甲基氯硅烷（TMCS）（体积比99∶1）的硅烷化试剂衍生后,在EI-SIM-MS模式下进行检测,内标法定量,雌二醇-D2与己烯雌酚-D8分别为雌二醇及己烯雌酚的定量内标。结果显示：DES和ES分别在1-500μg/L和1-250μg/L质量浓度范围内线性关系良好,相关系数均不低于0.999 1。对草鱼、对虾进行3个水平的加标回收实验（1.5,2.5,5.0μg/kg）,方法的平均回收率为86.1%-115%,相对标准偏差为0.43%-7.8%。DES和ES的检出限（LOD,S/N≥3）分别为0.3μg/kg和0.5μg/kg,低于欧盟食品中雌激素的最低执法限量（MRPL）（2-50μg/kg）以及美国食品中雌激素的残留限量（0.12-3μg/kg）,方法满足欧盟对水产品中雌激素残留的限量要求。
A QuEChERS sample preparation coupled with GC-MS was established for the simultaneous determination of diethylstilbestrol and estradiol residue in fish and shrimp.The QuEChERS（Quick,Easy,Cheap,Effective,Rugged and Safe） method was used for sample preparation.The sample was extracted with ethyl acetate as extraction solvent and MgSO4 as the sorbent,cleaned up by alumina-N,and then dried using a stream of nitrogen gas,derivatized with N,O-bis（trimethylsilyl） trifluoroacetamide（BSTFA） and trimethylchlorosilane（TMCS）（99∶1）,and finally determined by EI-SIM-MS.The estradiol and diethylstilbestrol were quantitatively analyzed by the internal standard method,using estradiol-D2 and diethylstilbestrol-D8 as the quantitative internal standard,respectively.Good linearities were obtained in the ranges of 1-500 μg/L for diethylstilbestrol and 1-250 μg/L for estradiol,with correlation coeffcients not less than 0.999 1.The average recoveries of diethylstilbestrol and estradiol in the grass carp and shrimp at three spiked levels of 1.5,2.5,5.0 μg/kg ranged from 86.1%to 115%,with relative standard deviations（RSD） of 0.43%-7.8%.The limits of detection（LOD,S/N≥3） for diethylstilbestrol and estradiol were 0.3 μg/kg and 0.5 μg/kg,respectively.This ensures a reliable determination at levels lower than the National Minimum Required Performance Limits（2-50 μg/kg for the xenohormones） of EU and the U.S.residue limits for veterinary drugs（0.12-3 μg/kg for natural hormones）.The method was simple, sensitive,rapid and accurate,and could be successfully used for the routine analysis of diethylstilbestrol and estradiol in fish and shrimp.
出处
《分析测试学报》
CAS
CSCD
北大核心
2015年第1期62-66,72,共6页
Journal of Instrumental Analysis
基金
国家农产品质量安全风险评估重大项目资助(901146)
