超高效液相色谱-串联质谱测定水产品中的卡巴氧、喹烯酮、乙酰甲喹及其代谢物

Determination of Residues of Carbadox,Quinocetone,Mequindox and Their Metabolites in Aquatic Products by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱法测定水产品中卡巴氧(CBX)、喹烯酮(QCT)、乙酰甲喹(MEQ)、喹啉-2-羧酸(QCA)、3-甲基喹啉-2-羧酸(MQCA)5种化合物残留的分析方法。样品分别采用乙酸乙酯-乙腈(50∶50)混合溶液、磷酸盐缓冲液分步提取,正己烷净化,以甲醇-乙腈(11∶3)混合溶液和0.1%甲酸溶液为流动相,经ACQUITYTM BEH C18色谱柱分离后进行LC-MS/MS多反应监测模式分析,外标法定量。结果表明,5种喹啉类化合物的响应值与其质量浓度在5～50μg/L范围内呈良好线性,相关系数均大于0.998,方法的定量下限为1.0μg/kg。在加标水平1.0～10μg/kg范围内,回收率为70%～108%,相对标准偏差(RSD)为2.5%～11%。该方法前处理过程简便快捷,回收率高,可满足实验室大量、快速分析的需求。

An ultra performance liquid chromatography- electrospray ionization triple-quadruple tandem mass spectrometric（ UPLC -ES1 MS/MS） method was established for the determination of residues of carbadox （CBX）, quinocetone （QCT）, mequindox （ MEQ）, quinoxaline-2-carboxylic acid （QCA） and 3-methylquinoxaline-2-carboxylie aeid（MQCA） in aquatic products. The samples were separately extracted with acetonitrile - ethyl acetate （50 ： 50） mixed solution and phosphate buffer, then purified with n-hexane. The separation of CBX, QCT, MEQ, QCA and MQCA was carried out on an ACQUITYTM BEH Cis column（ 1.7 μm, 2. 1 mmi. d. x 100 mm） using methanol - aeetronitril （ 11 ： 3） and 0. 1% formic acid as mobile phases. The target compounds were confirmed and quantified by MS -MS under multiple-reaction monitering（MRM） mode with the external standard method. The results showed that there were good linear relationships between peak area and concentrations of five quinoxalines in the range of 5 -50 μg/L, with correlation coefficients more than 0. 998 and limits of quantitation（LOQs） of 1.0 μg/kg. The recoveries at spiked levels of 1.0 -10 μg/kg ranged from 70% to 108% with relative standard deviations of 2.5% -11%. This method shortened the time of pre-treatment process, and the result was credible. It could satisfy the requirement of mass and fast analysis in the laboratory.