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用于测定食用动物组织中喹烯酮及其主要代谢物的简单快速萃取联用超高效液相色谱-串联质谱法

Simple and Fast Extraction-Coupled UPLC-MS/MS Method for the Determination of Mequindox and Its Major Metabolites in Food Animal Tissues.

作者信息

You Yanli, Song Liting, Li Yanshen, Wu Yongtao, Xin Mao

机构信息

College of Life Science, Yantai University , Yantai, Shandong 264005, People's Republic of China.

Hua Hai Property & Casualty Insurance Co., Ltd , Yantai, Shandong 264005, People's Republic of China.

出版信息

J Agric Food Chem. 2016 Mar 23;64(11):2394-404. doi: 10.1021/acs.jafc.5b05903. Epub 2016 Mar 15.

Abstract

This research described a sensitive and rapid UPLC-MS/MS method for the determination of mequindox and its six major metabolites in chicken muscle, chicken liver, swine muscle, and swine liver. Among the metabolites, carbonyl reduction-1,4-bisdesoxy-mequindox is novel. Target analytes could be extracted by ethyl acetate without any acidolysis or enzymolysis steps. After purification by a Bond Elut C18 cartridge, analysis was carried out by UPLC-MS/MS using positive ion multiple reaction monitoring (MRM) mode. Validation was performed in spiked samples, and mean recoveries ranged from 64.3 to 114.4%, with intraday and interday variations of less than 14.7 and 19.2%, respectively. The limit of detection (LOD) was <1.0 μg kg(-1), whereas the limit of quantification (LOQ) was <4.0 μg kg(-1). This procedure will help monitor mequindox residues in animal-derived food, and it will also facilitate further pharmacokinetics of mequindox.

摘要

本研究描述了一种灵敏且快速的超高效液相色谱-串联质谱法,用于测定鸡肉、鸡肝、猪肌肉和猪肝中喹乙醇及其六种主要代谢物。在这些代谢物中,羰基还原-1,4-双脱氧喹乙醇是新发现的。目标分析物可用乙酸乙酯提取,无需任何酸解或酶解步骤。经Bond Elut C18柱净化后,采用超高效液相色谱-串联质谱,在正离子多反应监测(MRM)模式下进行分析。在加标样品中进行了方法验证,平均回收率在64.3%至114.4%之间,日内和日间变化分别小于14.7%和19.2%。检测限(LOD)<1.0 μg kg⁻¹,而定量限(LOQ)<4.0 μg kg⁻¹。该方法将有助于监测动物源性食品中喹乙醇残留,也将有助于进一步研究喹乙醇的药代动力学。

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