食品与药品2024,Vol.26Issue(3) :199-205.DOI:10.3969/j.issn.1672-979X.2024.03.002

QuEChERS-超高效液相色谱-串联三重四极杆质谱联用法快速测定羊肉中氯霉素、甲砜霉素、氟苯尼考的残留量

Rapid Determination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Mutton by QuEChERS-UPLC-MS/MS

杜春艳 吴发旺 赖淼菊 吴劲竹 曹渟渟 邹晓莉
食品与药品2024,Vol.26Issue(3) :199-205.DOI:10.3969/j.issn.1672-979X.2024.03.002

QuEChERS-超高效液相色谱-串联三重四极杆质谱联用法快速测定羊肉中氯霉素、甲砜霉素、氟苯尼考的残留量

Rapid Determination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Mutton by QuEChERS-UPLC-MS/MS

杜春艳 1吴发旺 2赖淼菊 3吴劲竹 1曹渟渟 1邹晓莉4
扫码查看

作者信息

  • 1. 毕节医学高等专科学校,贵州 毕节 551700
  • 2. 毕节市疾病预防控制中心,贵州 毕节 551700
  • 3. 上海市普陀区疾病预防控制中心,上海 普陀 200333
  • 4. 四川大学 华西公共卫生学院,四川 成都 610000
  • 折叠

摘要

目的 建立 QuEChERS-超高效液相色谱-串联三重四极杆质谱法测定羊肉中氯霉素、甲砜霉素、氟苯尼考残留量的分析方法.方法 样品经研磨机匀浆后用乙腈提取,提取液经QuEChERS-1010,QuEChERS-0101净化,采用电喷雾负离子扫描,多反应监测模式,内标法定量.结果 氯霉素、甲砜霉素、氟苯尼考在4~50 μg/L范围内具有良好的线性关系,相关系数均大于0.998,3种药物在5.0,10.0,30.0 μg/kg浓度水平加标回收率在93.17%~109.91%范围内,相对标准偏差(RSD)为2.33%~6.14%.方法的检出限为0.01~0.03 μg/kg,定量限为0.02~0.09 μg/kg.结论 该方法具有操作简单,准确度和灵敏度高等特点,满足测定羊肉中氯霉素、甲砜霉素、氟苯尼考残留量的检测要求.

Abstract

Objective To establish an analytical method for the determination of chloramphenicol,thiamphenicol and florfenicol residues in mutton by QuEChERS-ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry(QuEChERS-UPLC-MS/MS).Methods The samples were homogenized by a grinder and extracted with acetonitrile.The extract was purified by QuEChERS-1010 and QuEChERS-0101,determined by UPLC-MS/MS and quantified by internal standard method.For detection,electrospray negative ion scanning and multiple reaction monitoring were adopted.Results Chloramphenicol,thiamphenicol and florfenicol showed good linear relationships in the range of 4-50 μg/L,with correlation coefficients above 0.998.At the concentrations of 5.0,10.0,30.0 μg/kg,the recoveries of three drugs were in the range of 93.17%-109.91%,and the relative standard deviations(RSDs)ranged from 2.33%to 6.14%.The limits of detection of the method were 0.01-0.03 μg/kg,and the limits of quantification were 0.02-0.09 μg/kg.Conclusion This method is simple,rapid,accurate and sensitive,and meets the detection requirements for the determination of chloramphenicol,thiamphenicol and florfenicol residues in mutton.

关键词

羊肉/氯霉素/甲砜霉素/氟苯尼考/QuEChERS-超高效液相色谱串联三重四极质谱法

Key words

mutton/chloramphenicol/thiamphenicol/florfenicol/QuEChERS-UPLC-MS/MS

引用本文复制引用

基金项目

2021年毕节市科学技术局毕节医学高等专科学校科学技术联合基金项目(毕科联合字yz[2021]4号)

出版年

2024
食品与药品
山东省生物药物研究院

食品与药品

CSTPCD
影响因子:0.537
ISSN:1672-979X
参考文献量17
段落导航相关论文