QuEChERS结合高效液相色谱串联质谱法检测猪肉中16种兽药残留量
Determination of 16 Kinds of Veterinary Drug Residues in Pork by QuEChERS Coupled with HPLC-MS/MS
陈楠楠 1陈秀明 1詹清 1揭小玲 1周阿容 1方东升1
作者信息
- 1. 福建省微生物研究所,福建 福州 350007
- 折叠
摘要
建立了一种QuEChERS前处理与高效液相色谱串联质谱法(HPLC-MS/MS)相结合同时检测猪肉中 16 种兽药残留的方法.样品采用水-0.1%甲酸乙腈经QuEChERS技术提取和净化后,在正离子多反应监测模式(multiple reaction monitoring,MRM)下进行分析测定.结果表明:16 种兽药在 2.0～100.0 μg·kg-1 的范围内有良好的线性关系(相关系数r＞0.9970);检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)的范围分别为 0.01～0.25 μg·kg-1、0.03～0.82 μg·kg-1;在猪肉样品中进行了 2、4、20 μg·kg-1 3 个不同浓度水平的加标试验,相对标准偏差RSD为 1.1%～9.0%,加标回收率在 70.4%～118.1%.该方法的重复性和回收率满足试验要求,灵敏度高,适用于猪肉中多种类兽药残留的分析检测.
Abstract
A method for the simultaneous determination of 16 veterinary drug residues in pork by using QuEChERS pretreatment combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established.The samples were extracted and purified by using the QuEChERS technology with water-0.1%formic acid acetonitrile,and then analyzed and determined in the positive ion multiple reaction monitoring(MRM)model.The results showed that:there was a good linear relationship among the 16 veterinary drugs in the range of 2.0-100.0 μg·kg-1(the correlation coefficient r＞0.9970).The limits of determination(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)ranged from 0.01 to 0.25 μg·kg-1 and from 0.03 to 0.82 μg·kg-1,respectively.The spiked experiments at three different concentration levels of 2,4 and 20 μg·kg-1 were carried out in the pork samples.The relative standard deviation(RSD)ranged from 1.1%to 9.0%,and the recovery rate ranged from 70.4%to 118.1%.The repeatability and recovery rate of the method met the test requirements,and the sensitivity was high,which was suitable for the analysis and detection of various veterinary drug residues in pork.
关键词
兽药残留/猪肉/高效液相色谱-串联质谱(HPLC-MS/MS)/QuEChERSKey words
Veterinary drug residues/Pork/High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/QuEChERS引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据