摘要
目的 建立QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速测定禽畜肉中157种农药残留的分析方法。方法 前处理采用QuEChERS方法,样品用1%甲酸乙腈提取,经无水硫酸镁、C18、N-丙基乙二胺粉(primary secondary amine,PSA)、多壁碳纳米管(multi-walled carbon nanotubes,MWCNTs)混合净化剂净化,经WatersAtlantisT3色谱柱分离,由加热电喷雾电离源(heatingelectronsprayionization,HESI)电离,在全扫描和数据依赖二级子离子全扫描(full scan/data-dependent full MS2,full scan/ddMS2)监测模式下检测,以一级质谱全扫描提取母离子精确质量数所得的色谱峰面积进行定量,以保留时间和数据依赖子离子扫描所得的二级子离子质谱图进行定性确证。结果 157种化合物的精确质量数偏差小于6.41×10-6,在各自线性范围内线性关系良好,相关系数大于0.9936,检出限为0.1~2.9μg/kg,定量限为0.2~8.8μg/kg,在3个不同添加水平下的平均回收率为60.6%~114.2%,相对标准偏差为0.2%~13.9%。结论 该方法操作简单、快速、灵敏,适用于禽畜肉中157种农药残留的定量筛查。
Objective To establish a method for rapid determination of 157 kinds of pesticide residues in livestock and poultry meat by QuEChERS combined with ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry.Methods The QuEChERS method was adopted for pretreatment,and the samples were extracted with 1% formic acid-acetonitrile and purified with a mixture of anhydrous magnesium sulfate,C18,primary secondary amine(PSA) and multi-walled carbon nanotubes(MWCNTs),separated on a Waters Atlantis T3 column,ionized by a heating electron spray ionization(HESI),and detected in the full scan/data-dependent full MS2(full scan/ddMS2) monitoring mode,the peak area of the chromatogram obtained by extracting the accurate mass number of the parent ion from the full scan of the first-stage mass spectrum was used for quantification,and the retention time and data were confirmed qualitatively by the two-stage daughter ion mass spectrum obtained by scanning the dependent daughter ions.Results The accurate mass deviation was less than 6.41×10-6,and the linearity was good within their respective linear ranges with correlation coefficient greater than 0.9936,limits of detection were 0.1-2.9 μg/kg,and limits of quantitation were 0.2-8.8 μg/kg,the average recoveries at the 3 different levels of addition were 60.6%-114.2%,and the relative standard deviations were 0.2%-13.9%.Conclusion This method is simple,rapid and sensitive,and is suitable for quantitative screening of 157 kinds of pesticide residues in livestock and poultry meat.
作者
张朋杰
张宪臣
李云松
林淑棉
胡仪光
曾苑嫦
黄碧嘉
ZHANG Peng-Jie;ZHANG Xian-Chen;LI Yun-Song;LIN Shu-Mian;HU Yi-Guang;ZENG Yuan-Chang;HUANG Bi-Jia(Zhongshan Customs Technology Center,Zhongshan 528403,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第16期5391-5400,共10页
Journal of Food Safety and Quality
基金
中山市社会公益与基础研究项目(2021B2060)。
关键词
QUECHERS
四极杆/静电场轨道阱高分辨质谱法
禽畜肉
农药残留
多壁碳纳米管
QuEChERS
quadrupole/electrostatic field orbitrap high resolution mass spectrometry
livestock and poultry meat
pesticide residues
multi-walled carbon nanotubes
