LC-MS/MS法同时测定动物源性食品中甲基睾丸酮和己烯雌酚的方法研究

Simultaneous Determination of Methyltestosterone and Diethylstilbestrol in Animal Products by LC-MS/MS

关键词:  甲基睾丸酮  己烯雌酚  液相色谱  质谱  动物源性食品

Key words:  Methyltestosterone  Diethylstilbestrol  Liquid Chromatography  Mass Spectrometry  Animal Products

摘要:

在研究了甲基睾丸酮和己烯雌酚的国内外检测进展的基础上，成功建立甲醇提取样品，LC-Alumina-A固相萃取柱净化提取液，使用C18液相色谱柱，甲醇+5 mmol/L乙酸铵（pH=4.5）=75+25(V/V)作为流动相，液相色谱-串联质谱进行多反应监测同时检测甲基睾丸酮和己烯雌酚雄雌两性激素类药物残留的高效液相色谱-串联质谱检测方法。在1.00~500 μg/L浓度范围内，甲基睾丸酮和己烯雌酚的响应值与浓度呈线性关系，相关系数（r）均大于0.999。方法检出限可达0.5 μg/kg。研究表明，方法适用于鸡鸭猪肉、虾肉、鸡猪肝脏等动物源性食品。

Abstract:

Study for progress in research on determination method internal and external of methyltestosterone and diethylstilbestrol was carried on afterwards, a method simultaneous determination of methyltestosterone and diethylstilbestrol based on liquid chromatography coupled to mass spectrometry was found, methanol was extraction reagent, sample extraction was purified by LC-Alumina-A minicolumn, chromatographic conditions included a C18 column with the mobile phase of V(methanol)+V(5mmol/Lammonium acetate,pH=4.5)=75+25. There was a good linear correlation in the range of 1.00~500 μg/L(r>0.999). The limit of detection was 0.5 μg/kg. Research showed that the method could apply to animal products such as chicken, duck, pork, shrimp, liver of chicken as well as liver of pig.