气相色谱-质谱法测定动物性食品中三种β-激动剂的残留量

建立了用气相色谱-质谱同时测定动物性食品中克伦特罗、沙丁胺醇和莱克多巴胺残留量的检测方法。样品用乙酸胺缓冲液匀浆,加入β-葡萄糖苷酸酶水解,用异丙醇-乙酸乙酯(40:60)萃取,有机相浓缩,经LC-SCX固相萃取柱进行分离,用4%氨化甲醇洗脱,洗脱液氮气吹干后,经N、O-双三甲基硅烷三氟乙酰胺(BSTFA)衍生后于气质联用仪上进行测定。检测采用选择性离子监控模式(SIM),以特征离子克伦特罗(86,262,243)、沙丁胺醇(86,369,440)和莱克多巴胺(250,267,502)定性,以试样峰(m/z86,m/z369,m/z250)的峰面积外标法定量。本方法检出限为克伦特罗和沙丁胺醇0.5ug/kg,莱克多巴胺2ug/kg;3种组分的线性相关系数均大于0.99。该方法的回收率为75%-98%,相对标准偏差为5%-14%。

The Detection of three β-Excitant Residue in Meats by GC/MS

A method was developed for the simultaneous determination of clenbuterol,salbutamol and ractopamine in meat by gas chromatography -mass spectrometry(GC/MS).The sample was extracted in acetate buffer of pH5.2 and the extraction was hydrolyzed by β-glucuronidase.The supernatant was passed through a SCX cation-exchange column and derivatized with N,O-bis(trimethylsiyl)trifluoroacetamide(BSTFA).The selected ion monitoring(SIM) method was used for detection,and the monitored ions were m/z86,262,243 for clenbuterol,m/z86,369,440 for salbutamol,m/z250,267,502 for ractopamine,respectively.Quantiation ions were selected at m/z86 for clenbuterol,m/z369 for salbutamol,m/z250 for ractopamine.The limits of detection were 0.5ug/kg for Clenbuterol and Salbutamol, 2ug/kg for ractopamine.The correfficients were better than 0.99 for the calibration curves for the drugs.The recoveries were 75%-98%,with relative standard deviations of 5%-14%.