通过式固相萃取-液相色谱-串联质谱法同时测定水产品中13种兽药残留  

Simultaneous Determination of 13 Kinds of Veterinary Drugs Residues in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry with Pass-Through Solid Extraction

作　　者：王勇跃 周鸿艳[1] 陈高尚[1] 徐云霞 WANG Yongyue;ZHOU Hongyan;CHEN Gaoshang;XU Yunxia(Jinhua Center for Disease Control and Prevention,Jinhua 321000,China)

机构地区：[1]金华市疾病预防控制中心,浙江金华321000

出　　处：《现代食品》2025年第3期200-206,共7页Modern Food

基　　金：金华市2022年度公益类科学技术研究计划项目(2022-4-223)。

摘　　要：目的:建立固相萃取-液相色谱-串联质谱法同时检测水产品中13种兽药残留的分析方法。方法:样品经1%甲酸-乙腈提取,Prime HLB柱净化,分别在正负离子模式下进样检测,以基质曲线外标法或内标法定量。结果:13种兽药在0.5~50.0μg·L^(-1)线性关系良好,相关系数r^(2)≥0.991,定量限在0.6~1.2μg·kg^(-1);在3个加标水平下,13种兽药的回收率在76.8%~109.2%,相对标准偏差在2.86%~11.20%。结论:该方法操作简便、准确性高、成本较低,适用于水产品中多种兽药残留的同时测定。Objective:To establish an analytical method for simultaneous detection of 13 veterinary drug residues in aquatic products using solid-phase extraction liquid chromatography tandem mass spectrometry.Method:The sample was extracted with 1%formic acid acetonitrile,purified on a Prime HLB column,and detected by injection in positive and negative ion modes.Quantification was performed using either the matrix curve external standard method or the internal standard method.Result:The linear relationship between 13 veterinary drugs is good in the range of 0.5~50.0μg·L^(-1),with a correlation coefficient r^(2)≥0.991 and a quantification limit of 0.6~1.2μg·kg^(-1);at three spiked levels,the recovery rates of 13 veterinary drugs ranged from 76.8%to 109.2%,with relative standard deviations between 2.86%and 11.20%.Conclusion:This method is easy to operate,highly accurate,and cost-effective,and is suitable for simultaneous determination of multiple veterinary drug residues in aquatic products.

关 键 词：兽药残留 水产品 固相萃取 液相色谱-串联质谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学]