Qu ECHERS-LC-MS/MS法测定牛奶中喹诺酮类药物

Determination of Quinolones in Milk by QuEChERS-High Performance Liquid Chromatography Tandem Mass Spectrometry

建立分散固相萃取-超高效液相色谱串联质谱同时测定牛奶中12种喹诺酮类药物残留的方法。牛奶样品中喹诺酮类药物经酸化乙腈提取,分散固相萃取净化,电喷雾离子源-三重四级杆串联质谱对喹诺酮类药物进行测定。12种喹诺酮类药物在5～200 ng/mL质量浓度范围内,其回归标准曲线方程的相关系数r为0.996 4～0.999 9。对空白牛奶添加5, 20和50μg/kg 3种浓度的喹诺酮类标准品,回收率为78.7%～96.3%,相对标准偏差(n=6)为1.99%～10.09%,方法检出限在1μg/kg以下。使用该方法对唐山本地牛奶样品进行检测,未发现有喹诺酮类药物检出。

A suitable method for routine analysis of quinolones in milk by Quick, Easy, Cheap, Effective, Rugged, and Safe(Qu ECh ERS) sample treatment method and ultra high performance liquid chromatography tandem mass spectrometry was developed and validated. Satisfactory recoveries calculated using an extracted matrix calibration curve ranged from 78.7% to 96.3% with RSD(n=6) less than 11% were obtained for the target compounds and the limits of detection for quinolongs were under 1 μg/kg in milk. The validated method was successfully applied to the determination of quinolones in milk samples from local supermarkets in Tangshan not detected in the analyzed samples.