QuEChERS-UPLC-MS/MS法同时测定青虾中27种兽药残留

李文杰 倪建秀 丁春晖 陈涛 陈桂芳

摘要 [目的]建立超高效液相色谱-串联质谱（UPLC-MS/MS）同位素内标法同时测定青虾中磺胺类、氟喹诺酮类、四环素类、酰胺醇类4大类27种兽药残留量的检测方法。[方法]青虾样品经86%（V/V）酸化乙腈（3%甲酸）-水溶液（含0.1 mol/L EDTA）提取后，提取液经分散固相萃取法净化，以UPLC-MS/MS测定，内标法定量。[结果]27种兽药在各自线性范围内呈良好的线性关系（R2≥0.99），磺胺类、氟喹诺酮类、酰胺醇类、四环素类的定量限分别为2.0、2.0、1.0、50.0 μg/kg，回收率在70.1%～110.0%，相对标准偏差（RSD）在0.2%～9.8%。[结论]该方法前处理简单、准确、对环境友好，适用于青虾中兽药残留的高通量快速检测分析。

关键词 QuEChERS-超高效液相色谱-串联质谱法;同位素内标法;兽药残留;青虾

中图分类号 TS254.7  文献标识码 A

文章编号 0517-6611（2021）24-0197-04

doi：10.3969/j.issn.0517-6611.2021.24.048

Simultaneous Determination of 27 Veterinary Drug Residues in Freshwater Shrimp by QuEChERS-UPLC-MS/MS

LI Wen-jie，NI Jian-xiu，DING Chun-hui et al （Quality Inspection Institute of Agricultural Products of Nanjing，Nanjing，Jiangsu 210036）

Abstract [Objective]To establish an ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） with isotope-labelled internal standard method，which was used to determine multiclass veterinary drugs residues simultaneously including sulfonamides，fluoroquinolones，tetracyclines and amphenicols in freshwater shrimp.[Method] The samples were extracted with 86% （V/V）acidified acetonitrile（3% formic acid）-water（containing 0.1 mol/L EDTA），then the extract was purified by dispersive solid phase extraction （DPSE）.The samples were determined by UPLC-MS/MS and quantified by internal standard method.[Result]27 kinds of veterinary drugs showed good linear relationship in their respective linear ranges （R2≥0.99）.The limits of quantification of sulfonamides，fluoroquinolones，amide alcohols and tetracyclines were 2.0，2.0，1.0，50.0 μg/kg，respectively.The recovery rates were 70.1%-110.0%.The relative standard deviations were 0.2%-9.8%.[Conclusion]The method is simple，accurate and environment-friendly，which is suitable for high-throughput rapid detection and analysis of veterinary drug residues in freshwater shrimp.

Key words QuEChERS-UPLC-MS/MS;Isotope internal standard method;Veterinary drug residue;Freshwater shrimp

基金项目

2018年度江苏省第五期“333工程”科研项目（BRA2018121）。

作者简介 李文杰（1980—）， 男， 江苏宜兴人，高级工程师，硕士，从事农产品质量安全检测与风险评估研究。通信作者，高级工程师，硕士，从事农产品质量安全检测工作。

收稿日期 2021-04-29

青虾，学名日本沼虾（Macrobrachium nipponense），是南京水产养殖的特色产业，养殖面积达4 666.67 hm2，产值超10亿元，规模仅次于螃蟹，尤其是2019年开始南京大面积推广养殖生长速度更快、抗病抗逆能力更强的新品种“太湖2号”，在科技创新、净化水环境、富民增收等方面發挥着重要作用[1]。近年来养殖者反映青虾出现散发性死亡[2]，需要合理使用兽药，防治消化道细菌感染等疾病[3]。因此，兽药残留成为青虾质量安全的一个关注热点。

目前，国内外动物性产品中兽药残……