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Determination of 5-nitroimidazoles and corresponding hydroxy metabolites i swine kidney by ultra-performance liquid chromatography coupled to electrospray tandem mass spectrometry

机译:高效液相色谱-电喷雾串联质谱法测定猪肾脏中的5-硝基咪唑及相应的羟基代谢物

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摘要

A rapid, sensitive and reliable multi-residue method for the simultaneous determination of four 5-nitroimidazoles (NHMs) 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 C_(18) column and was completed within 4 min 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 0.1-0.5 μgkg~(-1) respectively.
机译:建立并验证了同时测定猪肾脏中四种5-硝基咪唑(NHM)及其三种相应代谢产物的快速,灵敏和可靠的多残留方法。用乙酸乙酯从组织中提取目标化合物。将粗萃取物用己烷进行液-液分配,然后使用混合模式强阳离子交换柱进行固相萃取。色谱分离是在AcQuity BEH C_(18)色谱柱上完成的,每次进样均在4分钟内完成。在正电喷雾串联质谱法下的数据采集是通过应用多反应监测进行鉴定和定量的。强化样品的平均相对回收率介于83%至111%之间,变异系数低于12%。 NIIMs的检出限和定量限分别在0.05-0.5和0.1-0.5μgkg〜(-1)之间。

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