Xia Xi, Li Xiaowei, Ding Shuangyang, Zhang Suxia, Jiang Haiyang, Li Jiancheng, Shen Jianzhong
Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Anal Chim Acta. 2009 Apr 1;637(1-2):79-86. doi: 10.1016/j.aca.2009.02.008. Epub 2009 Feb 12.
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 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 microgkg(-1), respectively.
建立并验证了一种快速、灵敏且可靠的多残留方法，用于同时测定猪肾中四种5-硝基咪唑类药物（NIIMs）及其三种相应代谢物。用乙酸乙酯从组织中提取目标化合物。粗提物先用正己烷进行液液分配，然后使用混合模式强阳离子交换柱进行固相萃取。在AcQuity BEH C(18)柱上实现色谱分离，每次进样4分钟内完成。在正电喷雾串联质谱下，通过多反应监测进行数据采集，用于鉴定和定量。加标样品的平均相对回收率为83%至111%，变异系数低于12%。NIIMs的检测限和定量限分别在0.05 - 0.5和0.1 - 0.5 μgkg(-1)范围内。
