超高效液相色谱串联质谱法同时快速测定牛奶中不同类型的11种兽药残留  

Rapid and Simultaneous Determination of Several Classes of Veterinary Drug Residues in Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：方慧文 卢跃鹏 周原 江小明 杨永 

机构地区：[1]武汉产品质量监督检验所国家饮料及粮油制品质量监督检验中心(武汉),湖北武汉430048

出　　处：《分析测试学报》2013年第2期262-266,共5页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2012QK149)

摘　　要：建立了超高效液相色谱串联质谱测定牛奶中四环素类、青霉素类、磺胺类和泰乐菌素等11种兽药残留的检测方法。样品经乙腈超声提取后离心分离,上层清液稀释10倍后过0.2μm滤膜上机测定。在优化条件下,11种兽药在其线性范围内的相关系数均在0.998以上,定量下限(LOQ,S/N=10)为0.3～15μg/kg,在低、中、高3个水平下的加标回收率为81%～117%,相对标准偏差为0.6%～10.2%。方法用于实际牛奶样品中兽药残留量的测定,结果满意。An analytical method based on ultra performance liquid chromatography tandem mass spec- trometry （ UPLC - MS/MS） was developed for the rapid and simultaneous determination of 11 veterina- ry drug residues in milk. The analytes were extracted from the sample by ultrasonic bath in acetoni- trile and centrifuged. The supernatant liquid was diluted 10 times with mobile phase and filtered with a 0. 2 μm micro filter, and then analyzed by UPLC - MS/MS. Under the optimized conditions, the calibration curves for 11 veterinary drugs were linear with their correlation coefficients higher than 0. 998, and the limits of quantitation（LOQ, S/N= 10） ranged from 0. 3 μg/kg to 15 μg/kg. The mean recoveries at three spiked levels were between 81% and 117% with relative standard deviations of 0. 6% - 10. 2%. The proposed method was successfully applied in the determination of veterinary drug residues in milk with satisfactory results.

关 键 词：牛奶 多类兽药 超高效液相色谱串联质谱法 同时测定 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]