Shao Bing, Jia Xiaofei, Wu Yongning, Hu Jianying, Tu Xiaoming, Zhang Jing
Beijing Center for Disease Control and Prevention, Beijing 100013, China.
Rapid Commun Mass Spectrom. 2007;21(21):3487-96. doi: 10.1002/rcm.3236.
An ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC/MS/MS) method was developed to screen and confirm multi-class veterinary drug residues in pig tissues including pig kidney, liver and meat. Twenty-one drugs of two different classes including seven tetracyclines and four types of quinolones (quinoline, naphthyridine, pyridopyrimidine and cinoline) were determined simultaneously in a single run. The homogenized sample tissues were extracted with EDTA-McIlvaine buffer solution and further purified using a polymer-based Oasis HLB solid-phase extraction (SPE) cartridge. An ACQUITY UPLC BEH C18 column was used to separate the analytes followed by tandem mass spectrometry using an electrospray ionization source. MS data acquisition was performed in the positive ion multiple reaction monitoring mode, selecting two ion transitions for each target compound. Recovery studies were performed at different fortification levels. The overall average recoveries from pig muscle, kidney, and liver fortified with quinolones and tetracyclines at three levels ranged from 80.2 to 117.8% based on the use of matrix-fortified calibration with the coefficients of variation ranging from 2.1 to 17.8% (n=6). The limits of quantitation (LOQs) of quinolones and tetracyclines in different tissues ranged from 0.03-4.50 microg/kg and 0.16-10.00 microg/kg, respectively. The effects of the extraction solvent, SPE cartridge, elution solvent and sample matrix on the analyte recovery as well as the effects of the mobile phase composition and column temperature on the chromatographic behavior were also studied.
建立了一种超高效液相色谱-串联质谱（UPLC/MS/MS）方法，用于筛选和确证猪组织（包括猪肾、肝和肉）中的多类兽药残留。在一次进样中同时测定了两类不同的21种药物，包括7种四环素类药物和4种喹诺酮类药物（喹啉、萘啶、吡啶嘧啶和噌啉）。将匀浆后的样品组织用EDTA-麦氏缓冲液提取，再使用基于聚合物的Oasis HLB固相萃取（SPE）小柱进一步净化。采用ACQUITY UPLC BEH C18色谱柱分离分析物，然后使用电喷雾电离源进行串联质谱分析。质谱数据采集采用正离子多反应监测模式，为每种目标化合物选择两个离子跃迁。在不同的加标水平下进行回收率研究。基于基质加标校准，喹诺酮类和四环素类药物在猪肌肉、肾和肝中三个加标水平的总体平均回收率为80.2%至117.8%，变异系数为2.1%至17.8%（n = 6）。喹诺酮类和四环素类药物在不同组织中的定量限（LOQ）分别为0.03 - 4.50 μg/kg和0.16 - 10.00 μg/kg。还研究了萃取溶剂、SPE小柱、洗脱溶剂和样品基质对分析物回收率的影响，以及流动相组成和柱温对色谱行为的影响。
