超高压液相色谱-串联质谱法测定鱼组织中卡巴氧及喹乙醇代谢物
目的 建立鱼组织中卡巴氧代谢物喹恶啉-2-羧酸(QCA) 及喹乙醇代谢物3-甲基-喹恶啉-2-羧酸(MQCA)的超高压液相色谱-串联四极杆质谱(UPLC-MS/MS)残留分析方法。方法 样品在一定温度、Tris/HCL缓冲溶液作用下, 经蛋白酶酶解, 浓盐酸酸化, 乙酸乙酯提取, 提取液吹干后加入20%甲醇水溶解, 过PAX固相萃取柱净化、富集; 以乙腈-0.1%甲酸水为流动相, 经HSS T3色谱柱分离, 采用多反应监测(MRM)正离子模式进行检测。结果 QCA和MQCA定量限(LOQ)均为0. 5 μg/kg , 在0.5~5.0 μg/kg添加水平的平均回收率在93.1%~101.2%之间, 相对标准偏差为1.4%~5.5%。结论 本方法适用于鱼组织中卡巴氧及喹乙醇代谢物残留检测。
Objective An analytical method for the detection of quinoxaline-2-carboxylic acid (QCA) and 3-methyl-quinoxaline-2-carboxylic acid (MQCA), which were metabolites of carbadox and olaquindox, respectively, by ultra-pressure liquid chromatography -tandem quadrupole mass spectrometry (UPLC-MS/ MS) was established. Methods The enzymolysis of sample within Tris/HCl buffer under stable temperature was acidized by hydrochloric acid and extracted by ethyl acetate. The layer of ethyl acetate was evaporated to be nearly dry under a gentle stream of nitrogen. The residue was dissolved with methanol-water (1:4, v/v), and separated and purified by PAX cartridge. The objective compounds were separated using HSS T3 column with acetonitrile–water(0.1% formic acid) as mobile phase and analyzed by mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode(MRM). Results The LOQ for QCA and MQCA were both 0.5 μg/kg. The average recoveries were from 93.1% to 101.2% at the spiked level of 0.5~5.0 mg/kg with the relative standard deviation of 1.4%~5.5%. Conclusion The method is suitable for the detection of residual pollutant in fish tissues.
标题：超高压液相色谱-串联质谱法测定鱼组织中卡巴氧及喹乙醇代谢物
英文标题：Determination of metabolites of carbadox and olaquindox in fish tissue using ultra pressure liquid chromatography-tandem mass spectrometry
作者：
赵珊 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室
郭巧珍 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室
张晶 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室
邵兵 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室
中文关键词:喹恶啉-2-羧酸,3-甲基-喹恶啉-2-羧酸,超高压液相色谱-串联质谱法,
英文关键词:quinoxaline-2-carboxylic acid,methyl-3-quinoxaline-2-carboxylic acid,ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
发表日期：2012-11-15
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