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超高效液相色谱串联质谱法同时测定鸡组织中的唑类抗真菌药物

Simultaneous determination of azoles antifungal drugs in chicken tissues by ultra-performance liquid chromatography tandem mass spectrometry.

作者信息

Shang Nan, Zhang Jing, Shao Bing

机构信息

Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control.

出版信息

Anal Sci. 2013;29(12):1183-8. doi: 10.2116/analsci.29.1183.

Abstract

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of residues of enilconazole, parconazole, thiabendazole and its metabolite, 5-hydroxythiabendazole, in chicken tissues including liver, muscle and egg. Homogenized samples were extracted by acetonitrile, concentrated and purified by an Oasis MCX solid-phase extraction cartridge. Analysis of the target drugs was performed by liquid chromatography with an UPLCTM BEH C18 column, coupled with a tandem mass spectrometry (UPLC-MS/MS) operating in the positive multiple-reaction mode (MRM). Good linearity was obtained at concentrations of 0.10-100 μg kg(-1). The average recoveries of the analytes in chicken liver, muscle and egg at six fortification levels were in the range 93.6-119.5% with acceptable coefficients of variation (<14.8%). The detection capability (CCβ) of the analytes upon the method ranged from 0.05 to 138.1 μg kg(-1). This method was successfully applied in screening and confirming of target drugs in tens of real samples.

摘要

建立了一种超高效液相色谱 - 串联质谱(UPLC-MS/MS)方法,用于同时测定鸡组织(包括肝脏、肌肉和鸡蛋)中烯唑醇、戊康唑、噻苯达唑及其代谢物5-羟基噻苯达唑的残留量。将匀浆后的样品用乙腈提取,通过Oasis MCX固相萃取柱进行浓缩和净化。采用UPLCTM BEH C18柱进行液相色谱分析,并与以正离子多反应监测模式(MRM)运行的串联质谱(UPLC-MS/MS)联用,对目标药物进行分析。在0.10 - 100 μg kg(-1)浓度范围内获得了良好的线性关系。在六个加标水平下,鸡肝脏、肌肉和鸡蛋中分析物的平均回收率在93.6 - 119.5%之间,变异系数可接受(<14.8%)。该方法对分析物的检测能力(CCβ)范围为0.05至138.1 μg kg(-1)。该方法已成功应用于数十个实际样品中目标药物的筛查和确证。

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