液相色谱-串联质谱法测定鸡蛋中己烯雌酚的残留量  

Determination of diethylstilbestrol residues in eggs by liquid chromatography- tandem mass spectrometry

作　　者：谷晶[1] 权伍英[1] 

机构地区：[1]沈阳市疾病预防控制中心,辽宁沈阳110031

出　　处：《中国卫生检验杂志》2016年第2期199-201,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立液相色谱-串联质谱法快速检测鸡蛋中己烯雌酚的残留量。方法以乙腈为溶剂提取鸡蛋中的己烯雌酚,上清液用氮气吹干,加流动相溶解,正己烷脱脂后,液相色谱-电喷雾串联质谱负离子模式,选择反应监测(SRM)方式进行检测,定性离子对为m/z 267→m/z 251、m/z 267→m/z 237,其中m/z 267→m/z 251用于外标法定量。结果己烯雌酚的浓度为2.5 ng/ml^50 ng/ml时,线性关系良好,线性回归方程为y=4.32×104x-4.16×103,相关系数(r)为0.999 0。鸡蛋中己烯雌酚的定量检测限为0.5μg/kg(S/N=15)。在1.0μg/kg、5.0μg/kg、10.0μg/kg 3种加标水平下,己烯雌酚的平均回收率为88.0%~97.4%,相对标准偏差(RSD)为4.8%~8.7%。结论本法快速、灵敏、准确,可用于鸡蛋中己烯雌酚残留的痕量检测。Objective To develop a liquid chromatography- tandem mass spectrometry method for the determination of diethylstilbestrol residues in eggs. Methods The analyte was extracted with acetonitrile,the organic phase was dried under nitrogen and residues were redissolved in mobile phase,then defattened with hexane and analyzed by liquid chromatography- tandem mass spectrometry with electrospray ionization source operating in negative ion mode,reaction monitoring（ SRM） was selected to detect,the transitions m / z 267→m / z 251,m / z 267→m / z 237 used for monitoring product ions and m / z 267→m / z 251 used for quantification. Results When diethylstilbestrol concentration was among 2. 5 ng / ml- 50 ng / ml,the linear relationship was good,and the linear regression equation was y = 4. 32 × 104x- 4. 16 × 103 with correlation coefficientr = 0. 999 0. The limit of quantification for diethylstilbestrol in eggs was 0. 5 μg / kg（ S / N = 15）. The mean recoveries ranged from 88. 0% to 97. 4% at three levels for 1. 0 μg / kg,5. 0 μg / kg,10. 0 μg / kg and the relative standard derivations（ RSD） were among 4. 8%- 8. 7%.Conclusion The method is rapid,sensitive,accurate and suitable for rapid determination trace diethylstilbestrol residues in eggs.

关 键 词：液相色谱-串联质谱法 己烯雌酚 鸡蛋 

分 类 号：O657.63[理学—分析化学]