Shao Bing, Zhang Jing, Yang Yi, Meng Juan, Wu Yongning, Duan Hejun
Central Lab, Beijing Center for Disease Control & Prevention, Beijing 100013, China.
Rapid Commun Mass Spectrom. 2008 Nov;22(21):3427-33. doi: 10.1002/rcm.3740.
A simple, rapid, sensitive and specific method used to screen and confirm multi-class diuretics residues in whole bovine milk is described. Thirteen drugs of four different classes including carbonic anhydrase inhibitors, loop, thiazide and potassium-sparing diuretics were extracted from whole milk by acetonitrile followed by further purification with hexane. The analytes were separated using an ACQUITY UPLC BEH C18 column and detected by electrospray ionization tandem mass spectrometry (ESI-MS/MS). MS data acquisition was performed by a time-scheduled multiple reaction monitoring program, selecting two ion transitions for each target compound. The overall average recoveries based on matrix-fortified curves fortified with diuretics at three levels ranged from 80.6 to 108.8% with the coefficients of variation ranging from 2.6 to 19.7% (n = 6). The limits of quantitation (LOQs) of diuretics in bovine milk were 5.0 microg/kg for spironolactone and 0.5 microg/kg for other analytes, respectively.
本文描述了一种用于筛查和确证全脂牛奶中多类利尿剂残留的简单、快速、灵敏且特异的方法。通过乙腈从全脂牛奶中提取包括碳酸酐酶抑制剂、袢利尿剂、噻嗪类利尿剂和保钾利尿剂在内的四类共13种药物，随后用正己烷进一步纯化。使用ACQUITY UPLC BEH C18色谱柱分离分析物，并通过电喷雾电离串联质谱（ESI-MS/MS）进行检测。通过定时多反应监测程序进行质谱数据采集，为每种目标化合物选择两个离子跃迁。基于在三个水平添加利尿剂的基质强化曲线，总体平均回收率在80.6%至108.8%之间，变异系数在2.6%至19.7%之间（n = 6）。牛奶中利尿剂的定量限（LOQ）分别为螺内酯5.0微克/千克，其他分析物0.5微克/千克。
