超高效液相色谱串联质谱法检测鸡肉中5种雌激素残留  

Determination of Five Estrogens in Chicken by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：韩迪[1] 张艳[1] 周建于[1] 柏桦[1] 张敏[1] 王琦[1] 

机构地区：[1]昆明医科大学公共卫生学院,云南昆明650050

出　　处：《昆明医科大学学报》2014年第7期32-36,共5页Journal of Kunming Medical University

基　　金：云南省自然科学基金资助项目(2011FZ106)

摘　　要：目的 建立一种鸡肉中雌二醇、雌三醇、雌酮、17α-乙炔雌二醇、己烯雌酚5种雌激素残留的固相萃取结合高效液相色谱串联质谱的检测方法.方法 对色谱条件、萃取溶剂和固相萃取柱种类等条件进行优化选择.结果 以乙酸乙酯-甲醇（6∶1）为萃取溶剂,固相萃取柱HLB净化富集,采用ACQUITY BEH C18色谱柱进行分离,以乙腈-水溶液作为流动相进行梯度洗脱,在多反应监测模式下进行MS/MS的定性及定量分析.在此最佳条件下,方法显示出良好的线性,检出限为0.3 ～ 0.5 μg/kg,在添加水平为1～5 μg/kg范围内的平均回收率为80.0％～ 102.9％,相对标准偏差为6.9％ ～ 12.3％.结论 该方法适用于鸡肉中5种雌激素残留的检测,具有灵敏度高、操作简单快速的特点.Objective To establish an ultra performance liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometric （UPLC-ESI MS/MS） method for determination of 5 estrogens, including estradiol, estriol, estrone, 17α-ethinylestradiol and diethylstilbestrol in chicken. Method Analytical conditions including chromatography condition, extraction solvents and the type of solid phase extraction column were optimized. Results The estrogens were extracted by ethyl acetate and methanol （6：1） and cleaned up on a HLB solid phase extraction column, Separation of the estrogens was carried out by ACQUITY BEH C18 column on the condition of acetonitrile and water as the mobile phases. Finally, quantified by MS/MS under multiple reaction monitoring （MRM） mode. the target compounds were confirmed and On the optimized conditions, the methods showed good linearity and the limits of detection （LOD） was 0.3- 0.5 μg/kg. At spiked concentration of 1-5 μg/kg , the average recovery and RSD were 80.0 -102.9% and 6.9%-12.3% respectively. Conclusion The developed method is fast, sensitive and simple and suitable for the determination of 5 selected estrogens in chicken.

关 键 词：超高效液相色谱串联质谱 雌激素 动物性食品 鸡肉 

分 类 号：R155.5[医药卫生—营养与食品卫生学]