Development of a rapid method for the determination and confirmation of nitroimidazoles in six matrices by fast liquid chromatography-tandem mass spectrometry
Development of a rapid method for the determination and confirmation of nitroimidazoles in six matrices by fast liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.jpba.2012.02.013
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发表时间：
2012-05-01
影响因子：
3.4
通讯作者：
Farkas, Szilvia
中科院分区：
文献类型：
--
作者：
Toelgyesi, Adam;Sharma, Virender K.;Farkas, Szilvia
建立了血浆、牛奶、肌肉、鸡蛋、蜂蜜和饲料样品中的硝基咪唑、甲硝唑(MNZ)、硝唑(RNZ)和二甲基咪唑(DMZ)及其羟基代谢物MNZ-OH和2-羟甲基-1-甲基-5-硝基咪唑(HMNNI)的快速液相色谱-串联质谱(LC-MS/MS)分析方法。对每个基质使用相同的样品净化程序，包括一种新的聚合物Strata-SDB柱上的固相萃取(SPE)。色谱柱为Kinetex XB C-18核壳型高效液相色谱柱，流动相为0.1%甲酸-水-甲醇(88/12，v/v，pH 2.6)，流速为0.7ml/min。该方法的主要优点是分析时间仅为3min，比已报道的其他高效液相色谱方法缩短了约3~10倍。开发的方法使用矩阵综合内部验证策略进行了验证。研究了LC-MS/MS分析中的基质效应。结果表明，所开发的方法成功地应用于猪肉认证标准物质，并在2011年的一次熟练测试中引起猪血浆。(C)2012爱思唯尔B.V.保留所有权利。
A rapid liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed to identify and to quantify nitroimidazoles, metronidazole (MNZ), ronidazole (RNZ) and dimetridazole (DMZ) and their corresponding hydroxy metabolites, MNZ-OH and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMNNI) in plasma, milk, muscle, egg, honey and feed samples. The same sample clean-up procedure including a novel solid-phase extraction (SPE) on polymeric Strata-SDB cartridges was used for each matrix. The analytes were separated on Kinetex XB C-18 core-shell type HPLC column using iso-cratic elution mode with a mobile phase containing 0.1% formic acid in water/methanol (88/12, v/v, pH 2.6) at a flow rate of 0.7 ml/min. The main advantage of the developed method is that the analysis time of only 3 min, which is about three to ten times shorter than in other reported HPLC methods. The developed method was validated using a matrix-comprehensive in-house validation strategy. The matrix effect of LC-MS/MS analysis was also investigated. Results are presented from the successful application of the developed method to an incurred pork meat certified reference material and to incur porcine plasmas in a proficiency test in year 2011. (C) 2012 Elsevier B.V. All rights reserved.