UPLC-MS/MS测定动物源性食品中3种二苯乙烯类激素残留

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

关键词:  二苯乙烯类,动物源性食品,超高效液相色谱-串联质谱

Key words:  stilbenes, products of animal origin, ultra performance liquid chromatography- tandem mass spectrometry

摘要:

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0.1 µg/kg，定量限均为0.5 µg/kg；在1.0µg/kg ，1.5 µg/kg，2.0 µg/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%。本方法分析速度快，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。

Abstract:

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 µg/kg，1.5 µg/kg，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 legisla-tion．The method adapts to the determination of stilbenes residues in different products of animal origin.