UPLC-MS/MS法测定金沙江水域鱼体中卡巴氧及喹乙醇代谢物  

Determination of metabolites of carbadox and olaquindox in fish tissues of Jinsha River by UPLC-MS/MS

作　　者：孙卓然[1] 田金凤[2] 尚远宏[2] SUN Zhuoran;TIAN Jinfeng;SHANG Yuanhong(Hohhot Center for Disease Prevention and Control,Hohhot 010070,China;College of Medicine,Panzhihua University,Panzhihua 617000,China)

机构地区：[1]呼和浩特市疾病预防控制中心,内蒙古呼和浩特010070 [2]攀枝花学院医学院,四川攀枝花617000

出　　处：《中国酿造》2020年第11期179-182,共4页China Brewing

基　　金：西华大学食品生物技术省高校重点实验室开放课题(szjj2017-110);攀枝花市社会发展科技计划项目(2018CY-S-28)。

摘　　要：采用同位素内标-超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)法测定金沙江攀枝花江段6种常见鱼中卡巴氧代谢物喹恶啉-2-羧酸(QCA)和喹乙醇代谢物3-甲基-喹恶啉-2-羧酸(MQCA)的残留量。样品经过预处理,采用ZORBAX SB-C18色谱柱分离,以0.1%甲酸水-乙腈为流动相进行梯度洗脱;采用电喷雾-正离子多反应监测模式(MRM)检测,同位素内标法定量。结果表明,QCA和MQCA的质量浓度为2.0~100.0 ng/mL时,线性关系良好(R>0.999),回收率为91.4%~100.4%,精密度试验结果相对标准偏差(RSD)为6.3%~11.5%,定量限为0.2μg/kg,检出限为0.05μg/kg。该方法灵敏度及准确度良好,能满足6种常见鱼的组织中卡巴氧及喹乙醇代谢物残留分析的要求。The quinoxaline-2-carboxylic acid(QCA)and 3-methyl-quinoxaline-2-carboxylic acid(MQCA)residues which were metabolites of carbadox and olaquindox in 6 common fish tissues in the Panzhihua section of the Jinsha River were determined by UPLC-MS/MS with isotope internal standards.The samples were pretreated,separated on a ZORBAX SB-C18 column with gradient elution using a mobile phase made up of 0.1%formic acid water solution and acetonitrile,detected by electrospray positive ion multiple reaction monitoring(MRM)mode,and quantified with isotope internal standard method.The results showed that the linear relationship of QCA and MQCA was good in the range of mass concentration 2.0-100.0 ng/ml(R>0.999).The recovery rate was 91.4%-100.4%,the relative standard deviation(RSD)of precision test result was 6.3%-11.5%,and the detection limit and quantitation limit were 0.2μg/kg and 0.05μg/kg,respectively.The method with good sensitivity and accuracy could meet the requirements for the analysis of residues of carbadox and olaquindox metabolites in 6 common fish tissues.

关 键 词：超高效液相色谱串联三重四极杆质谱法 喹恶啉-2-羧酸 3-甲基-喹恶啉-2-羧酸 鱼 

分 类 号：Q657.7[生物学—生物物理学]