Determination of 5-nitroimidazoles and corresponding hydroxy metabolites in swine kidney by ultra-performance liquid chromatography coupled to electrospray tandem mass spectrometry.
Determination of 5-nitroimidazoles and corresponding hydroxy metabolites in swine kidney by ultra-performance liquid chromatography coupled to electrospray tandem mass spectrometry.
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DOI：
10.1016/j.aca.2009.02.008
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发表时间：
2009-04
影响因子：
6.2
通讯作者：
X. Xia;Xiaowei Li;S. Ding;Suxia Zhang;Haiyang Jiang;Jiancheng Li;Jianzhong Shen
中科院分区：
文献类型：
--
作者：
X. Xia;Xiaowei Li;S. Ding;Suxia Zhang;Haiyang Jiang;Jiancheng Li;Jianzhong Shen
建立了同时测定猪肾中4种5-硝基咪唑及其3种代谢物的快速、灵敏、可靠的多残留方法。用乙酸乙酯从组织中提取感兴趣的化合物。粗提物经正己烷液液分流，固相萃取后采用混合模式强阳离子交换柱萃取。在AcQuity BEH c18色谱柱上进行色谱分离，每次进样在4min内完成。电喷雾串联质谱法的数据采集采用多重反应监测进行鉴定和定量。强化样品的平均相对回收率为83% ~ 111%，变异系数小于12%。niim的检出限为0.05 ~ 0.5μgkg - 1，定量限为0.1 ~ 0.5μgkg - 1。
A rapid, sensitive and reliable multi-residue method for the simultaneous determination of four 5-nitroimidazoles (NIIMs) and their three corresponding metabolites in swine kidney was developed and validated. The compounds of interest were extracted from tissues with ethyl acetate. The crude extracts were subject to liquid–liquid partition with hexane followed by solid-phase extraction using mixed-mode strong cation-exchange column. Chromatographic separation was achieved on an AcQuity BEH C18column and was completed within 4min for each injection. Data acquisition under positive electrospray tandem mass spectrometry was performed by applying multiple reaction monitoring for both identification and quantification. Mean relative recoveries from fortified samples ranged from 83% to 111%, with coefficients of variation lower than 12%. The limits of detection and quantification for the NIIMs were in the range of 0.05–0.5 and 0.1–0.5μgkg−1, respectively.