多壁碳纳米管改进QuEChERS-液相色谱-串联质谱法测定豆类中12种酰胺类杀菌剂残留量  

Determination of 12 amide fungicides in legumes by multi-walled carbon nanotubes QuEChERS-liquid chromatography-tandem mass spectrometry

作　　者：李巧莲 罗景阳 张宏宏 王岩松 宣彤 蒋笑妍 LI Qiao-lian;LUO Jing-yang;ZHANG Hong-hong;WANG Yan-song;XUAN Tong;JIANG Xiao-yan(Shenyang Food and Drug Inspection Institute,Shenyang 110136,Liaoning,China;School of Public Health,Shenyang Medical College,Shenyang 110034,Liaoning,China;College of Food Science,Shenyang Agricultural University,Shenyang 110866,Liaoning,China)

机构地区：[1]沈阳市食品药品检验所,辽宁沈阳110136 [2]沈阳医学院公共卫生学院,辽宁沈阳110034 [3]沈阳农业大学食品学院,辽宁沈阳110866

出　　处：《粮食与油脂》2023年第1期157-162,共6页Cereals & Oils

基　　金：国家市场监督管理总局科技计划项目(2020MK134);沈阳市科学技术局科技计划项目(22-322-3-37)。

摘　　要：建立基于多壁碳纳米管改进分散固相萃取净化技术(QuEChERS),结合液相色谱-串联质谱法(LC-MS/MS),测定豆类中12种酰胺类杀菌剂残留量。结果表明:改进的QuEChERS最佳条件为无水MgSO4添加量800 mg、PSA添加量200 mg、HC-C18添加量100 mg、MWCNTs添加量25 mg;在此条件下测得的12种酰胺类杀菌剂在0.1~2.5μg/L范围内均具有良好的线性关系,相关系数均大于0.99;方法检出限为0.05~2.00μg/kg,定量限为0.2~5.0μg/kg;加标实验平均回收率为70.7%~115.0%,相对标准偏差为0.4%~7.4%。该方法操作快捷,净化效果好,灵敏度高,适用于豆类中酰胺类杀菌剂残留量的分析。An improved dispersive solid-phase extraction purification technology(QuEChERS)based on multi-walled carbon nanotubes was established to determine the residues of 12 amide fungicides in legumes by LC-MS/MS.The results showed that the optimal conditions for the improved QuEChERS were anhydrous MgSO_(4) addition 800 mg,PSA addition 200 mg,HC-C_(18) addition 100 mg and MWCNTs addition 25 mg.Under these conditions,the 12 amide pesticides showed good linearity in the mass concentration range of 0.1-2.5μg/L,and correlation coefficients were above 0.99.The limits of detection and quantification were 0.05-2.00μg/kg and 0.2-5.0μg/kg,respectively.The average recoveries were 70.7%-115.0% and the relative standard deviations were 0.4%-7.4%.This method had the advantages of fast operation,good purification efficiency and was sensitive,suitable for the determination of amide fungicide residues in legumes.

关 键 词：多壁碳纳米管 分散固相萃取净化技术 液相色谱-串联质谱法 酰胺类杀菌剂 

分 类 号：TS207.5[轻工技术与工程—食品科学]