通过式净化-液相色谱-串联质谱快速筛查水产品中15类107种兽药多残留的方法研究  

Simultaneous determination of 15 categories and 107 kinds of veterinary drugs in aquatic products by pass-through purification and liquid chromatography-tandem mass spectrometry

作　　者：孙晓杰[1] 高金芳 李兆新[1] 郭萌萌[1] 邢丽红[1] 孙伟红[1] 翟毓秀[1] 姜薇 SUN Xiao-Jie;GAO Jin-Fang;LI Zhao-Xin;GUO Meng-Meng;XING Li-Hong;SUN Wei-Hong;ZHAI Yu-Xiu;JIANG Wei(Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality,Ministry of Agriculture,Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Qingdao 266071,China;Weifang Institute of Inspection on Product Quality,Weifang 261000,China)

机构地区：[1]农业部水产品质量安全检测与评价重点实验室,中国水产科学研究院黄海水产研究所,青岛266071 [2]潍坊市产品质量检验所,潍坊261000

出　　处：《食品安全质量检测学报》2020年第22期8240-8246,共7页Journal of Food Safety and Quality

基　　金：山东省农业重大应用技术创新项目(SF1405303301);中国水产科学研究院基本科研业务费项目(2020TD71);中国水产科学研究院黄海水产研究所基本科研业务费项目(20603022019001)。

摘　　要：目的建立水产品基质中15类包含107种药物多残留的快速筛查方法。方法通过多溶剂分步提取-通过式净化,结合液相色谱-串联质谱仪,在MRM模式下正、负离子同时扫描监测水产品,实现水产品中15类107种药物多残留的快速筛查,并用于实际水产样品中药物残留含量的测定。结果所有药物在35 min内分离良好,方法线性范围为0.1~200 ng/mL,相关系数均大于0.995;检出限为0.1~5.0μg/kg (S/N>3),定量限为0.3~10μg/kg(S/N>10);回收率为40.0%~120%,相对标准偏差均小于15%。结论方法的准确性和灵敏度较高,重现性好,适合水产基质中药物多残留的高通量、快速筛查,能够满足国家限量法规的要求。Objective To establish a rapid screening method for 15 categories containing 107 drug residues in aquatic product substrates. Methods The aquatic products were extracted by multi-solvent step and pass-through-purified, combined with liquid chromatography-tandem mass spectrometer, and the positive and negative ions were scanned and monitored simultaneously in MRM mode. The rapid screening of 15 categories and 107 kinds of drug residues in aquatic products were realized and applied to the determination of drug residues in actual aquatic samples. Results All the drugs were well separated within 35 mins. The linear ranges of the method were 0.1-200 ng/mL, and the correlation coefficients were greater than 0.995. The limits of detection were 0.1-5.0 μg/kg(S/N>3), and the limits of quantitation were 0.3-10 μg/kg(S/N>10). The recoveries were 40.0%-120%, and the relative standard deviations were less than 15%. Conclusion The method has high accuracy, sensitivity and good reproducibility, which is suitable for high throughput and rapid screening of drug residues in aquatic substrate, and can meet the requirements of national limit regulations.

关 键 词：水产品 兽药 多残留 快速筛查 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]