CAJ | 학술논문

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0.5μg/kg ,在0.5~5.0μg/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.
목적건립어조직중잡파양대사물규악람-2-최산(QCA)급규을순대사물3-갑기-규악람-2-최산(MQCA)적초고압액상색보-천련사겁간질보(UPLC-MS/MS)잔류분석방법.방법양품재일정온도、Tris/HCL완충용액작용하,경단백매매해,농염산산화,을산을지제취,제취액취간후가입20%갑순수용해,과PAX고상췌취주정화、부집;이을정-0.1%갑산수위류동상,경HSS T3색보주분리,채용다반응감측(MRM)정리자모식진행검측.결과 QCA화MQCA정량한(LOQ)균위0.5μg/kg ,재0.5~5.0μg/kg첨가수평적평균회수솔재93.1%~101.2%지간,상대표준편차위1.4%~5.5%.결론본방법괄용우어조직중잡파양급규을순대사물잔류검측.
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 0.5μg/kg. The average recoveries were from 93.1%to 101.2%at the spiked level of 0.5~5.0μg/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.