UPLC-MS/MS法测定动物源食品中42种兽药残留  

Determination of 42 drugs Residues in Animal Derived food by UPLC-MS/MS

作　　者：张雪娇 于雷[2] 陈洋 曹忠君 田亚平[2] 

机构地区：[1]辽宁省铁岭市畜产品安全检测站,辽宁铁岭112000 [2]中国动物疫病预防控制中心,北京102609

出　　处：《现代畜牧兽医》2015年第4期9-22,共14页Modern Journal of Animal Husbandry and Veterinary Medicine

摘　　要：本研究建立动物源性食品中10种β-受体激动剂类药物、14种喹诺酮类药物和18种磺胺类药物的UPLC-MS/MS分析方法,为食品安全监测提供数据支撑。样品用三氯乙酸乙腈提取并去除蛋白质,目标药物用Waters Acquity UPLC BEH C18柱（100 mm×2.1 mm,1.7μm）分离,以0.05%甲酸水溶液和甲醇为流动相进行梯度洗脱,流速：0.25 m L/min,柱温：30℃,进样量：10μL。结果显示,喹诺酮及磺胺类药物在1.0~100.0 ng/m L的浓度范围内呈良好的线性关系,相关系数均大于0.996;检测限为0.5 ng/m L,定量限为1.0 ng/m L。对于β-受体激动剂类药物在1.0~100.0 ng/m L的浓度范围内呈良好的线性关系,相关系数（r）均大于0.992;检测限为0.5 ng/m L,定量限为1.0 ng/m L。经方法学验证,本方法专属性好,简便准确快速,适用于动物源性食品中兽药残留的检测。To develop a UPLC- MS/MS analysis method for the determination of 10 beta-agonists, 14 quinolones and 18 sulfonamides so as to provide data support for guaranteeing food safety. The samples were extracted with trichlo- roacetic acid and acetonitrile. Waters Acquity UPLC BEH C18 （100 mm×2.1 mm,1.7μm）） was used as separation col- umn. And the mobile phase was 0.05% formic acid in water-methanol for gradient elution. The flow rate was 0.25 mL/ rain, the column temperature was 30 ℃, the injection volume was 10 L. Quinolone and sulfa drugs in the concentra- tion range of 1.0- 100.0 ng/mL showed a good linear relationship,and the linear correlation coefficient was above 0.996, the detection-limit was 0.5 ng/mL, the quantification limit was 1.0 ng/mL. The linear relationship for beta-agonists in range of 1.0- 100.0 ng/mL was also well, the linear correlation coefficient was above 0.992, the detection limit was 0.5 ng/mL, the quantification limit was 1.0 ng/mL. The methodology validation shows that the established method is specif- ic, simple, accurate and rapid, which can be used to determine 42 drugs.

关 键 词：β-受体激动剂类药物 喹诺酮类药物 磺胺类药物 高效液相色谱串联质谱 

分 类 号：S859.84[农业科学—临床兽医学]