浙江农业学报 ›› 2023, Vol. 35 ›› Issue (1): 175-183.DOI: 10.3969/j.issn.1004-1524.2023.01.19

• 农产品质量安全 • 上一篇    下一篇

加速溶剂萃取-超高效液相色谱-串联质谱法测定婴幼儿配方乳粉中17种磺胺类药物残留

吉小凤1(), 王小骊1, 吕文涛1, 周忠静2, 吴钰潇3, 杨华1,*()   

  1. 1.浙江省农业科学院 农产品质量安全与营养研究所,浙江 杭州 310021
    2.农产品质量安全危害因子与风险防控国家重点实验室,浙江 杭州 310021
    3.浙江工业大学 化学工程学院,浙江 杭州 310014
  • 收稿日期:2021-08-19 出版日期:2023-01-25 发布日期:2023-02-21
  • 通讯作者: *杨华,E-mail:yanghua@zaas.ac.cn
  • 作者简介:吉小凤(1974—),女,河北唐山人,硕士,副研究员,研究方向为农产品质量安全。E-mail: jxfzjsnky@163.com
  • 基金资助:
    国家重点研发计划政府间合作项目(2019YFE01039000);江山市“一县一品一策”示范县创建(ZJNY2021001-012)

Determination of 17 sulfonamides in infant formula by accelerated extraction and ultra-high performance liquid chromatography/mass spectrometry

JI Xiaofeng1(), WANG Xiaoli1, LYU Wentao1, ZHOU Zhongjing2, WU YUxiao3, YANG Hua1,*()   

  1. 1. Institute of Agro-Product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
    2. State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-Products, Hangzhou 310021, China
    3. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China
  • Received:2021-08-19 Online:2023-01-25 Published:2023-02-21

摘要:

建立了加速溶剂萃取(ASE)-超高效液相色谱-串联质谱法(UHPLC-MS/MS) 测定婴幼儿配方乳粉中17种磺胺类药物残留的方法,并对方法的线性、灵敏度、回收率及基质效应等进行验证分析,同时将该方法应用于市场采集的婴幼儿配方乳粉样品中磺胺类药物残留进行分析和确证。试验结果表明,17种磺胺类药物在0.5~100 μg·kg-1范围内呈线性,决定系数均大于0.998,不同添加浓度下的回收率为75.3%~103.6%,相对标准偏差 (RSD) 均小于11.0%, 基质效应为0.4~1.0, 检出限为0.1~3.0 μg·kg-1,定量限为0.3~10 μg·kg-1。该方法具有萃取便捷、灵敏度和准确度高等特点,可同时对婴幼儿配方乳粉中17种磺胺类药物残留进行测定。

关键词: 加速溶剂萃取, 超高效液相色谱-串联质谱法, 乳粉, 磺胺类药物

Abstract:

A method for the determination of 17 sulfonamides residues in infant formula by accelerated solvent extraction (ASE) and ultra-high performance liquid chromatography/mass spectrometry (UHPLC-MS/MS) was developed. The linearity, sensitivity, recovery rate and matrix effect of the method were verified. Meanwhile, the screening analysis for 17 sulfonamides in infant formula collected from the market was carried out. The results showed that the linearity of sulfonamides were in the range of 0.5-100 μg·kg-1, and the correlation coefficient was greater than 0. 998, the recoveries were 75.3%-103.6%, the relative standard deviation was less than 11.0%, the matrix effect was 0.4-1.0, the detection limit for sulfonamides in infant formula was 0.1-3.0 μg·kg-1, and the limit of quantification (LOQ) was 0.3-10 μg·kg-1. The developed method has the merits for convenient extraction, high sensitivity and accuracy, and the method can simultaneously determine 17 sulfonamides residues in infant formula.

Key words: accelerated solvent extraction (ASE), ultra-high performance liquid chromatography/mass spectrometry (HPLC-MS/MS), infant formula, sulfonamides

中图分类号: