胡飞杰，张 露^*，徐美玲，王晓丽，马 雯^*，顾慧丹，叶沐阳，陆秀凤，陈良茜

（南京市产品质量监督检验院，南京市质量发展与先进技术应用研究院，江苏南京 210019）

摘要：针对不同形态的乳品基质中11种兽药残留（氯霉素类、地塞米松、林可霉素、替米考星、喹诺酮类和磺胺类），采用超高效液相色谱-三重四极杆串联质谱（ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry，UPLC-MS/MS）分析，对比考察了增强型脂质去除固相萃取柱（Captiva EMR-Lipid）净化与传统固相萃取小柱的净化效果，并考察了多种形态的乳制品在不同称样量下的回收率。结果表明，Captiva EMR-Lipid具有有效的脂质净化性能，可以明显减少目标分析物的损失及基质影响，从而获得更高的回收率、精密度及质谱检测灵敏度。应用Captiva EMR-Lipid结合UPLC-MS/MS分析的方法简便、快速，适用于乳品中8种兽药（氯霉素、氟苯尼考、甲砜霉素、林可霉素、替米考星、诺氟沙星、恩诺沙星和环丙沙星）残留的快速定量检测分析。

关键词：超高效液相色谱-三重四极杆串联质谱法；牛奶；兽药残留；快速筛查

中图分类号：TS207.3   文献标识码：A   文章编号：1674-506X（2022）02-0124-0006

Analysis of 8 Veterinary Drug Residues in Dairy Products by a New Solid Phase Extraction Column Combined with Ultra Performance Liquid Chromatography-triple Quadrupole Tandem Mass Spectrometry

HU Feijie, ZHANG Lu^*, XU Meiling, WANG Xiaoli, MA Wen^*, GU Huidan, YE Muyang，LU Xiufeng, CHEN Liangqian

（Nanjing Institute of Product Quality Inspection, Nanjing Institute of Quality Development and Advanced Technology Application, Nanjing Jiangsu 210019, China）

Abstract：As for 11 veterinary drugs (Chloramphenicols, dexamethasone, lincomycin, tilmicosin, quinolones and Sulfonamides) in different dairy products, ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC- MS/MS) is employed to compare the purification results between with enhanced column of Captiva EMR-Lipid and with the traditional solid phase extraction. The recovery ratios of the dairy products in many forms with different sample quantities are then investigated. Captiva EMR- Lipid exhibits effective lipid purification performance, and then the loss of target analyte and matrix effect can be obviously inhibited, and thus higher recovery, precision, and mass spectrometry detection sensitivity can be realized. It is easy and effective to employ the UPLC-MS/MS cooperated with the Captiva EMR-Lipid to rapidly and quantitatively analyze 8 veterinary drugs (chloramphenicol,  florfenicol, thiamphenicol, lincomycin, tilmicosin, norfloxacin, enrofloxacin and ciprofloxacin) in the dairy products.

Keywords：ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry; milk; veterinary drug residues; rapid screening

doi：10.3969/j.issn.1674-506X.2022.02-019

收稿日期：2021-09-15

基金项目：国家重点研发计划项目（2019YFF0216700）；国家市场监督管理总局科技计划项目（2020MK139）；江苏省市场监督

管理局科技计划项目（KJ21125040）；江苏省重点研发计划（社会发展）面上项目（BE2020627）

作者简介：胡飞杰（1979-），男，硕士，高级工程师。研究方向：食品及食品添加剂监测分析。

*通信作者：张露（1988-），女，博士，工程师。研究方向：食品中兽药残留监测分析；马雯（1989-），女，硕士，工程师。研究方向：食品及食品添加剂分析。

引用格式：胡飞杰,张露,徐美玲,等.新型固相萃取结合超高效液相色谱-三重四极杆串联质谱分析乳品中8种兽药残留[J].食品与发酵科技,2022,58(2):124-129.