猪肉和鸡肉中11种同化激素残留超高效液相色谱-串联质谱法测定  

Determination of Eleven Anabolic Steroids in Pork and Chicken by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张家华 方炳虎[2] 王敏儒[1] ZHANG Jia-hua;FANG Bing-hu;WANG Min-ru(Foshan University,Foshan,Guangdong,528000,China;South China Agricultural University,Guangzhou,Guangdong,510642,China)

机构地区：[1]佛山科学技术学院,广东佛山528000 [2]华南农业大学,广东广州510642

出　　处：《动物医学进展》2021年第4期48-53,共6页Progress In Veterinary Medicine

基　　金：农业部农业行业标准制定和修订项目(181721301092371)。

摘　　要：为建立用于猪肉、鸡肉中睾酮、甲睾酮、黄体酮等11种同化激素残留量检测的超高效液相色谱-串联质谱法,将鸡肉、猪肉组织样品通过甲醇-乙腈(1∶1,v/v)提取和C18固相萃取柱净化处理后,进行梯度洗脱,电喷雾电离,在正离子、多反应监测模式下进行检测分析。结果表明,11种目标分析物在试验浓度范围内线性良好,相关系数均大于0.99;在10、20、50μg/kg浓度水平下,猪肉中11种同化激素的平均回收率为74.3%~101.1%,鸡肉中11种同化激素的平均回收率为70.1%~97.4%。11种同化激素在猪肉、鸡肉中检测限和定量限分别为0.1μg/kg~0.5μg/kg和0.3μg/kg~1μg/kg,变异系数均小于15%。所建立的方法灵敏度高,特异性强,可适用于猪肉、鸡肉中睾酮等11种同化激素的残留检测分析。To establish a reliable and sensitive ultra performance liquid chromatography-tandem mass spectrometry method for the detection of eleven anabolic steroids in pork and chicken,the tissue samples were extracted with methanol-acetonitrile(1∶1,v/v)and purified with C18 solid phase extraction column,and then separated in a gradient program,and analyzed by mass spectrometry equipped with an electrospray ionization source,operating in the positive ionization modes,and performed in the multiple reaction monitoring using external standards.Results showed that good linearity could be observed among eleven anabolic steroids with coefficients higher than 0.99.The average recoveries of eleven anabolic steroids in pork was about 74.3%-101.1%and about 70.1%-97.4%in chicken at the additive concentrations of 10μg/kg,20μg/kg,and 50μg/kg.The limits of detection and quantification of eleven anabolic steroids in pork and chicken were about 0.1μg/kg-0.5μg/kg and 0.3μg/kg-1μg/kg,respectively,with the coefficient of variation less than 15%.The proposed method is sensitive and specific and can be used in the residue detection and analysis of eleven anabolic hormones in pork and chicken.

关 键 词：同化激素 残留 猪肉 鸡肉 超高效液相色谱-串联质谱 

分 类 号：S859.793[农业科学—临床兽医学]