QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中30种抗寄生虫类药物残留
Determination of 30 Kinds of Antiparasitic Drugs in Animal-derived Foods by QuEChERS-UPLC-MS/MS
冯丽凤 1黄芊 1叶梦薇 1黄永辉 1黄燕 1林浩学 1梁敏 1许晖1
作者信息
- 1. 福建省产品质量检验研究院国家加工食品质量监督检验中心,福建福州 350002
- 折叠
摘要
目的:采用超高效液相色谱-串联质谱法,建立测定动物源性食品中 30种抗寄生虫类药物残留的方法.方法:样品经乙腈、1%氨水乙酸乙酯提取,经QuEChERS净化.净化后采用Waters ACQUITY UPLCTM BEH C18 色谱柱分离,10 mmol/L甲酸铵(含 0.1%甲酸)水溶液-乙腈:甲醇(50:50,v:v)为流动相进行梯度洗脱,电喷雾离子源正负离子切换多反应监测(Multiple Reaction Monitoring,MRM)模式下进行检测,基质匹配外标法定量.结果:在优化的条件下,30种抗寄生虫类药物在各自的线性范围内线性良好,决定系数(r2)均大于 0.99;回收率为 70.1%～111%;相对标准偏差在 0.10%～9.1%之间(n=6);方法检出限为 0.001～0.3 μg/kg之间,方法定量限在 0.004～1 μg/kg.结论:该方法灵敏、准确,具有良好的重复性和稳定性,可用于动物源性食品中多种抗寄生虫药物残留的检测.
Abstract
Objective:A method for determining the residues of 30 antiparasitic drugs in animal-derived food using ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Methods:The samples were extracted with acetonitrile and 1%ammonia acetic ether and purified by QuEChERS.After purification,Waters ACQUITY UPLCTM BEH C18 column was used for separation,and a gradient elution of 10 mmol/L ammonium formate(containing 0.1%formic acid)aqueous solution,acetonitrile:methanol(50:50,v:v)was performed as the mobile phase.Detection was carried out using electrospray ionization(ESI)in both positive and negative ion modes using multiple reaction monitoring(MRM).Matrix-matched external standard quantification was used.Results:Under the optimized conditions,the 30 antiparasitic drugs showed good linearity within their respective linear ranges,with coefficient of determination(r2)greater than 0.99.The recoveries ranged from 70.1%to 111%,and the relative standard deviations were between 0.10%and 9.1%(n=6).The method detection limit ranged from 0.001 to 0.3 μg/kg,and the method quantification limit ranged from 0.004 to 1 μg/kg.Conclusion:The method is sensitive,accurate,and exhibits good repeatability and stability,making it suitable for detecting various antiparasitic drug residues in animal-derived food.
关键词
抗寄生虫药物/超高效液相色谱-串联质谱法/QuEChERS/动物源性食品/药物残留Key words
antiparasitic drugs/ultra-high-performance liquid chromatography-tandem mass spectrometry/QuEChERS/animal derived food/drug residues引用本文复制引用
基金项目
福建省市场监督管理局科技项目(FJMS2020004)
国家市场监督管理总局科技计划项目(2021MK054)
出版年
2024
国家科技期刊平台
NSTL
万方数据