鱼虾中喹乙醇及其代谢标示物的同步检测

Simultaneous determination of olaquindox and its metabolic marker in fish and shrimp

建立了液相色谱-串联三重四极杆质谱(LC-MS/MS)同步检测鱼虾中的喹乙醇(OLA)及其代谢标示物3-甲基喹噁啉-2-羧酸(MQCA)的方法。样品用0.1 mol/L的盐酸37℃水解16 h,水解液乙腈萃取,正己烷去脂,HLB固相萃取柱净化,LC-MS/MS分析,内标法定量。结果表明,OLA和MQCA在1.00~200μg/L范围内呈良好线性,相关系数均在0.999以上,方法检出限为0.50μg/kg,定量限为1.00μg/kg。在1.00、2.00、10.0μg/kg加标水平下,OLA平均回收率为84.5%~107.0%,MQCA平均回收率为74.0%~106.0%,相对标准偏差(RSD)均小于10%。该方法灵敏度高,操作简单,可适用于鱼虾肌中喹乙醇及其代谢标示物的同步检测。

A liquid chromatography–tandem mass spectrometric method was developed to determine olaquindox(OLA)and its metabolic marker 3-methylquinoxaline-2-carboxylic acid(MQCA)simultaneously in fish and shrimp.Sample was hydrolyzed with 0.1 mol/L hydrochloric acid for 16 h at 37℃,the hydrolytic solution was extracted with acetonitrile,defatted with n-hexane and purified with HLB solid-phase extraction cartridge,detected by liquid chromatography–tandem mass spectrometry(LC-MS/MS).The quantification was done by internal standard method.The analysts showed good linearity within the range 1.00~200μg/L.The correlation coefficient(r)was greater than 0.999.The limit of detection was 0.50μg/kg and the limit of quantitation was 1.00μg/kg.At the three spiked levels of 1.0,2.0 and 10.0μg/kg,the average recoveries of OLA were in range 84.5%~107.0%and MQCA in range 74.0%~106.0%.The relative standard deviations were below 10%.The proposed method is sensitive and easy to operate,it is suitable for detection of OLA and MQCA in fish and shrimp muscle tissues.