UPLC-MS/MS测定动物源性食品中3种二苯乙烯类激素残留

建立了动物源性食品中二苯乙烯类激素己烯雌酚、己烷雌酚和双烯雌酚残留的超高效液相色谱-串联质谱（UPLC-MS/MS）测定法。样品均质后,采用β-葡萄糖醛酸酶/芳基硫酸酯酶酶解,叔丁基甲基醚提取,硅胶固相萃取柱净化。采用UPLC-MS/MS多反应监测（MRM）模式检测,内标法定量。方法对己烯雌酚、己烷雌酚和双烯雌酚的检出限均为0.1μg/kg,定量限均为0.5μg/kg;在1.0、1.5、2.0μg/kg三个浓度添加水平,总体平均回收率为75.8%-110.0%,总体相对标准偏差为3.3%-13.2%。本法分析速度快,灵敏度高,重现性好,各项技术指标均满足国内外相关法规要求,可用于各种动物源性食品中二苯乙烯类激素己烯雌酚、己烷雌酚和双烯雌酚残留的快速检测。

Determination of Stilbenes Residues in Products of Animal Origin by Ultra Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the determination of stilbenes residues including diethylstilbestrol, hexestrol and dienoestrol in products of animal origin. The homogenized samples were hydrolysised with beta-glucuronidase and the analytes were extracted with tert-butyl methyl ether. Then the extract was cleaned by silica solid phase extraction cartridge. Quantification of the three analytes was achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) using internal standard method. Detection limits and quantification limits of UPLC-MS/MS for the three analytes were all 0.1 μg/kg and 0.5 μg/kg. The overall recovery varies from 75.8%～110.0% at the spiked level of 1.0,1.5,2.0 μg/kg, and the relative standard deviation (RSD) of the method was from 3.3%～13.2%. The method was reliable, sensitive and reproducibility, its performance can meet the requirements of the domestic and international legislation.The method adapts to the determination of stilbenes residues in different products of animal origin.