超高效液相色谱-串联质谱法同时测定鸡肉和猪肉中的喹烯酮、喹乙醇及其主要代谢物
Simultaneous determination of mequindox, quinocetone, and their major metabolites in chicken and pork by UPLC-MS/MS.
作者信息
Li Yanshen, Liu Kaili, Beier Ross C, Cao Xingyuan, Shen Jianzhong, Zhang Suxia
机构信息
College of Life Science, Yantai University, Yantai 264005, PR China.
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, PR China; Beijing Fengtai District Animal Health Inspection, Beijing, PR China.
出版信息
Food Chem. 2014 Oct 1;160:171-9. doi: 10.1016/j.foodchem.2014.03.094. Epub 2014 Mar 26.
This report presents a UPLC-MS/MS method for determination of mequindox (MEQ), quinocetone (QCT) and their 11 metabolites in chicken and pork samples. Following extraction process with acetonitrile-ethyl acetate, acidulation, and re-extraction with ethyl acetate in turn, target analytes were further purified using C18 solid phase extraction (SPE) cartridges for UPLC-MS/MS analysis. Validation was processed with mean recoveries from 69.1% to 113.3% with intra-day relative standard deviation (RSD) <14.7%, inter-day RSD <19.2%, and limit of detection between 0.05 and 1.0 μg/kg for each analytes. The verified method was successfully applied to the quantitative determination of commercial samples. This developed procedure will help to control food animal products with MEQ and QCT residues, and facilitate further pharmacokinetic and residue studies of similar quinoxaline-1,4-dioxide veterinary drugs.
本报告介绍了一种用于测定鸡肉和猪肉样品中喹烯酮（MEQ）、喹乙醇（QCT）及其11种代谢物的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。依次用乙腈-乙酸乙酯萃取、酸化，再用乙酸乙酯萃取后，目标分析物使用C18固相萃取（SPE）柱进一步纯化，用于UPLC-MS/MS分析。验证结果显示，平均回收率为69.1%至113.3%，日内相对标准偏差（RSD）<14.7%，日间RSD<19.2%，各分析物的检测限在0.05至1.0μg/kg之间。该验证方法成功应用于商业样品的定量测定。此开发的方法将有助于控制含有MEQ和QCT残留的食用动物产品，并促进对类似喹喔啉-1,4-二氧化物兽药的进一步药代动力学和残留研究。
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