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超高效液相色谱-质谱联用法测定水产品中喹乙醇代谢物残留量
引用本文:梅光明,郑斌,陈雪昌,张小军,孙秀梅,朱婧睿,蔡慧萍.超高效液相色谱-质谱联用法测定水产品中喹乙醇代谢物残留量[J].浙江水产学院学报,2010(3):254-259.
作者姓名:梅光明  郑斌  陈雪昌  张小军  孙秀梅  朱婧睿  蔡慧萍
作者单位:浙江海洋学院海洋与渔业研究所,浙江海洋水产研究所。浙江舟山316100
基金项目:农业部标准制定项目(2009C32008)
摘    要:建立了水产品中喹乙醇代谢物残留量的超高效液相色谱-质谱联用测定方法。样品经乙酸乙酯提取、液液萃取净化后吹干,流动相定容,经超高效液相色谱分离后进入串联质谱检测器。采用电喷雾正离子,多反应监测(MRM)模式检测,内标法定量。方法的检出限为1μg/kg,浓度在2~100 ppb范围内,线性良好(r=0.999),添加浓度1~20μg/kg下,不同水产品基质的回收率在80%~100%之间,相对标准偏差(RSD)小于10%。

关 键 词:喹乙醇代谢物  3-甲基喹噁林-2-羧酸  MQCA  超高效液相色谱-质谱法

Study on Determination of MQCA in Aquatic Product by UPLC-MS/MS
Institution:MEI Guang-ming,ZHENG Bin,CHEN Xue-chang,et al(Marine and Fishery Research Institute of Zhejiang Ocean University,Marine Fishery Research Institute of Zhejiang Province,Zhoushan 316100,China)
Abstract:A ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for determination of methyl-3-quinoxaline-2-carboxylic acid(MQCA) in acquatic product.Samples were extracted with ethyl acetate and further purified with liquid-liquid extraction,then the solvent was vaporized and MQCA was dissolved with mobile phase.Analytical identification and quantification were performed using multiple reaction monitoring(MRM) with electrespray ionization in positive mode.The detection limit was 1 μg/kg.It was linearly ranged from 2 to100 ppb with the correlation coefficient of 0.999.The average recoveries for different matrices were 80%-100% when the concentration of MQCA ranged from 1 to 20 μg/kg and the relative standard deviation was less than 10%.
Keywords:olaquindox metabolite residues  methyl-3-quinoxaline-2-carboxylic acid  MQCA  UPLC-MS/MS
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