气质联用法检测水产品中己烯雌酚含量并用液相色谱串联质谱验证

摘要

Aeconomical analytical method by chromatograph-mass spectrometer was developed for the diethylstilbestrol (D E S) in aquatiCproducts. Thesamples were extracted with acetiCether, purified by HLB extraction column, and get derivative reaction with B ST FA-T mCS in pyridines at 80°C. Theextract was separated on an agilent H P-5mS capillary column (30m×0.25mm, 0.25 μm) and detected with high resolution mass spectrometry in SImmode (m/z:383, 397, 412, 413). T here ware two derivative compounds, Cis-D E S-(O T mS) 2 and T rans-D E S-(O T mS) 2 displayed by chromatogramand the T rans-D E S-(O T mS)2 was the quantitative compound for D E S. Theresults showed that high correlation coefficients (R=0.995) were obtained within their respective linear ranges when have Arange of 5-180 μg/kg. Theaverage recoveries for 1μg/kg, 2μg/kg, 5μg/kg spiked levels ranged from90.15% to 92.82% with R SD s of 6.7%-9.3% . The positive samples were verified by LC-mS/mS with R B AX SB-C18 column for higher reliability.%改进了水产品中己烯雌酚的检测方法。样品用乙酸乙酯提取，HLB固相萃取柱净化，BSTFA-TMCS吡啶溶液80°C衍生；经过HP-5MS（30m×0.25mm，0.25μm）毛细色谱柱分离，再经过单四级杆质谱仪选择离子扫描（m/z：383、397、412、413）确定两种结构的衍生物，用气质联用仪检测其衍生物从而间接检测己烯雌酚。以反式衍生物做定量物质，在5-180μg/kg浓度范围获得良好线性（R=0.995）；3个添加浓度（1、2、5μg/kg）下的平均回收率为90.15%-92.82%，标准偏差为6.7%-9.3%。阳性样品经过乙酸乙酯提取后吹干，HLB固相萃取柱净化，甲醇定容后，用配备RBAXSB-C18柱（2.1×150mm，3.5μm）的高分辨率液相色谱串联质谱仪进行验证，确保检测的可靠性。