液相色谱串联质谱法测定动物组织中大环内酯类残留量

Determination of macrolide residues in animal tissues by liquid chromatography tandem mass spectrometry

采用高效液相色谱-电喷雾串联质谱仪（LC -ESI-MS-MS），建立猪肉中林可霉素、竹桃霉素、替米考星、泰乐菌素、克林霉素、吉他霉素、交沙霉素等7种大环内酯类药物残留的检测方法，试验中猪肉中大环内酯类抗生素的残留用乙腈提取，以罗红霉素作为内标，提取液用正己烷去除脂肪后浓缩，再用磷酸盐溶液溶解后，经HLB固相萃取柱净化，甲醇洗脱，洗脱液浓缩定容至1mL ，供液相色谱-串联质谱法测定，内标法定量。本方法采用10μg/kg ，20μg/kg ，100μg/kg ，3个添加浓度，每个浓度6个平行样品，上述7种大环内酯类药物残留的回收率在75％～100％，相对偏差在1.51％～5.48％。

A method was established for the determination of seven kinds of macrolide drug residue in pork ,seven kinds of macrolide drug were lincomycin ,oleandomycin ,tilmicosin ,tylosin ,clindamycin , kitasamycin ,josamycin. The sample was extracted with acetonitrile. With roxithromycin as an internal standard ,extract was washed with n-hexane to remove fat and then concentrated ,phosphate solution dis-solved ,cleaned by the HLB solid phase extraction （SPE） ,methanol eluate and concentrated to volume 1mL ,for liquid chromatography-tandem mass spectrometry determination ,internal standard. This method uses 10μg/kg ,20μg/kg ,100μg/kg ,3 spiked concentration ,each concentration six parallel samples .The seven kinds of macrolide drug residues recovery is 75%-100% ,the relative deviation is 1.51%-5.48%.