摘要
以草鱼、南美白对虾、中华绒鳌蟹为样品,建立了喹烯酮（QCT）和喹赛多（CYA）及其主要代谢物脱二氧喹烯酮（BDQCT）、3-甲基喹啉-2-羧酸（MQCA）、脱二氧喹赛多（BDCYA）和喹啉-2-羧酸（QCA）多残留的高效液相色谱-串联质谱（HPLC-MS/MS）确证检测方法。组织样品经乙腈-乙酸乙酯（1∶1）、盐酸溶液分步提取,Oasis MAX固相萃取柱净化,以甲醇、乙腈和0.1%甲酸溶液为流动相,经Waters XBridge C18色谱柱分离后,采用HPLC-MS/MS仪进行测定。采取正离子选择反应监测模式检测,外标法定量。结果表明,喹烯酮和喹赛多及其主要代谢物的响应值与其质量浓度在2-500μg/L范围内线性关系良好。在加标浓度为5-50μg/kg范围内,6种待测物的平均回收率为76.3%-94.2%,相对标准偏差为4.2%-11.7%。方法的检出限为0.5-1.6μg/kg,定量下限为2.0-5.0μg/kg。该方法适用于水产品中QCT和CYA及其主要代谢物残留的确证检测和同时定量分析。
A high performance liquid chromatography - tandem mass spectrometric （ HPLC - MS/MS） method was established for the determination of the residual quinoeetone （QCT）, cyadox （CYA）, bidesoxyquinocetone （ BDQCT）, methyl-3-quinoxaline-2-carhoxylic acid （ MQCA ）, bidesoxycyadox （BDCYA） and quinoxaline-2-carboxylic acid （QCA） in aquatic products. Samples were extracted with acetonitrile- ethyl acetate （1 ： 1 ） and hydrochloric acid solution, then cleaned up on a MAX solid-phase extraction cartridge. The separation of QCA, BDQCT, MQCA, CYA, BDCYA and QCT was carried out on a Waters XBridge C18 column using methanol, acetonitrile and 0. 1% fomic acid as mobile phase. The identification of six analytes was performed by selective reaction monitoring in positive electrospray ionization, and the quantification was done by the external standard method. The calibration curves of six analytes were linear in the range of 2 - 500 μg/L. At the fortified levels of 5 -50 μg/kg, the recoveries ranged from 76.3% to 94.2% , with RSDs of 4.2% to 11.7% . The limits of detection （LOD） were in the range of 0. 5 - 1.6 μg/kg and the limit of quantitation （LOQ） were 2.0 -5.0 μg./kg. The results showed that the method could be used to analyze simulta- neously QCT, CYA and their metabolites residues in aquatic products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第12期1535-1541,共7页
Journal of Instrumental Analysis
基金
上海市青年人才成长计划(沪农青字【2015】第3-10号)
关键词
水产品
喹烯酮
喹赛多
代谢物
高效液相色谱-串联质谱(HPLC-MS/MS)
aquatic products
quinocetone （QCT）
cyadox （CYA）
metabolites
high perform-ance liquid chromatography - tandem mass spectrometry（ HPLC - MS/MS）
