方志娟 李晓芹 丁洪流 何新叶 金萍 王伟

摘要 [目的]建立超高效液相色谱-串联质谱法（UPLC-MS/MS）定量检测动物源性食品中16种非甾体消炎类兽药残留量的方法。[方法]样品用甲酸-水-乙腈混合溶液提取，净化后经C18色谱柱分离，UPLC-MS/MS法测定。[结果]样品由基质匹配标准曲线进行定量，所检测的16种非甾体消炎药在1～200 ng/g线性关系良好（R2>0.995）。分别添加1倍定量限、2倍定量限和10倍定量限3个水平的混合标准溶液进行回收率试验，各个浓度水平加标回收率在70%～105%，相对标准偏差（RSD）均在15%以下（n=6）。[结论]该方法简便、稳定、准确，具有良好的重现性，适用于测定动物源性食品中16种非甾体消炎类兽药残留量。

关键词 超高效液相色谱-串联质谱法;非甾体消炎类药;动物源性食品;兽药残留

中图分类号 TS 207  文献标识码 A  文章编号 0517-6611（2021）21-0211-04

doi：10.3969/j.issn.0517-6611.2021.21.054

开放科学（资源服务）标识码（OSID）：

Determination of 16 Non-steroidal Anti-inflammatory Veterinary Drugs Residues in Animal-origin Foods by UPLC-MS/MS

FANG Zhi-juan  LI Xiao-qin  DING Hong-liu2 et al

（1.Suzhou Institute for Food Control， Suzhou，Jiangsu 215104;2. Suzhou Institute of Product Quality Supervision and Inspection， Suzhou，Jiangsu 215104）

Abstract [Objective]To establish a method for the quantitative determination of 16 non-steroidal anti-inflammatory drugs （NSAIDs） in animal-origin foods by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. [Method]The samples were extracted with a mixture of formic acid-water-acetonitrile. After purification， the samples were separated by C18 column and quantitatively detected by UPLC-MS/MS. [Result]The samples were quantified by matrix matching standard curves. The 16 NSAIDs had good linear relationships in the range of 10-200 ng/mL （R2 >0.995）. The mixed standard solutions of   2 and 10 times of the limits of quantification （LOQ） were added respectively for the recovery experiments，the recovery rates of each concentration level were 70%-105%， and the relative standard deviation （RSD） were all less than 15%（n=6）. [Conclusion]The method is simple， stable， accurate and reproducible. It is suitable for the determination of 16 NSAIDs in animal-origin foods.

Key words Ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）; Non-steroidal anti-inflammatory drugs （NSAIDs）;Animal-origin foods;Veterinary drug residue

基金項目 苏州市科技计划项目（SS2019039，SS202038）。

作者简介 方志娟（1987—），女，江苏南通人，工程师，硕士，从事食品检测与质量管理工作。*通信作者，工程师，硕士，从事食品安全检测与分析工作。

收稿日期 2021-06-23

近年来，兽药在养殖和畜牧业中使用的越来越广泛。动物源性食品中的兽药残留一方面会限制养殖和畜牧业的健康发展，另一方面，随着动物体内兽药的积累和对外排泄量的增多，会对生态环境造成严重影响，进一步还会对人类食品安全以及身体健康造成威胁[1]。非甾体类消炎药（non-steroidal anti-inflammatory drugs，NSAIDs）具有抗炎、退热、止痛、抗风湿、抗凝效果[2]，临床上主要用于风湿性疾病、心血管疾病、肿瘤类疾病和慢性疼痛等。每天……