南美白对虾中喹乙醇及其代谢物3-甲基-喹恶啉-2-羧酸残留的高效液相色谱-串联质谱检测  

Determination of residual olaquindox and methyl-3-quinoxaline-2-carboxylic acid in penaeus vannamei by HPLC-MS / MS

作　　者：郭霞[1] 孙振中[1] 戚隽渊[1] 孙建华[1] 黄雪玲[1] 刘琴[1] 丁义[1] 

机构地区：[1]上海市水产研究所,上海200433

出　　处：《中国农业大学学报》2014年第1期156-160,共5页Journal of China Agricultural University

基　　金：2013年无公害农产品质量安全监测项目资金(农财发[2013]86号)

摘　　要：以南美白对虾为试验材料,建立了喹乙醇(OLA)及3-甲基-喹恶啉-2-羧酸(MQCA)多残留的高效液相色谱-串联质谱(HPLC-MS/MS)确证检测法.组织样品经2 mol/L盐酸提取,Oasis HLB固相萃取柱净化,采用HPLC-MS/MS仪进行测定.质谱检测采用正离子选择反应监测模式,外标法定量.样品中OLA和MQCA质量分数分别为2～200和4～200 μg/kg时,线性关系良好;当质量分数分别为2～50和4～50 μg/kg时,平均回收率为93.9％～103.2％,变异系数为6.3％～11.5％.OLA及MQCA的检测限分别为0.5和1.0 μg/kg,定量限分别为2.0和4.0 g/kg.该方法灵敏、准确、简便、快速,适于南美白对虾中OLA及MQCA残留的同时定量分析和确证检测.A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) determination of Olaquindox and methyi-3-quinoxaline-2-carboxylic acid in Penaeus vannamei muscle was established.Samples were extracted with 2 mol/L hydrochloric acid and clean-up was performed on a HLB solid-phase extraction cartridge.The residues were detected by HPLC-MS/MS.The identification was performed by selective reaction monitoring in positive electrospray ionization.The quantification was done by external standard method.Calibration curves were linear for OLA and MQCA in samples at 2-200 and 4-200μg/kg respectively.At the fortified levels of 2-50 and 4-50 μg/kg,the recoveries ranged from 93.9％ to 103.2％,coefficents of variation (CV) ranged from 6.3％ to 11.5％.The limit of detection (LOD) of OLA and MQCA was 0.5 and 1.0 μg/kg respectively and the limit of quantitation (LOQ) was 2.0 and 4.0 μg/kg respectively.The results show that the method is sensitive,accurate,convenient and quick,which can be used to analyze simultaneously OLA and MQCA residues in penaeus vannamei muscle.

关 键 词：南美白对虾 喹乙醇 3-甲基-喹恶啉-2-羧酸 残留 高效液相色谱-串联质谱 

分 类 号：S968.229[农业科学—水产养殖] O657.63[农业科学—水产科学]