多壁碳纳米管QuEChERS-液相色谱-串联质谱法测定粮谷中14种酰胺类杀菌剂残留量  

Determination of 14 Amide Pesticides in Cereals by Multi-Walled Carbon Nanotubes Qu ECh ERS-Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李巧莲 宣彤 袁帅 王岩松 罗景阳 蒋笑妍 肖舒元 LI Qiaolian;XUAN Tong;YUAN Shuai;WANG Yansong;LUO Jingyang;JIANG Xiaoyan;XIAO Shuyuan(Shenyang Food and Drug Inspection Institute,Shenyang 110136,China;School of Public Health,Shenyang Medical College,Shenyang 110034,China;College of Food Science,Shenyang Agricultural University,Shenyang 110866,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：《食品科技》2023年第5期300-307,共8页Food Science and Technology

基　　金：辽宁省市场监督管理局科技计划项目(2022ZC023);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的QuEChERS净化方法,结合液相色谱-串联质谱法测定粮谷中14种酰胺类杀菌剂。样品经乙腈提取,无水硫酸镁、N-丙基乙二胺、多壁碳纳米管和十八烷基硅烷键合硅胶净化,在多反应监测模式下用正离子扫描,使14种目标化合物在Symmetry C_(18)色谱柱上分离,外标法定量。在0.10~2.50μg/L范围内14种目标化合物具有良好的线性关系,相关系数(r)均大于0.99,方法检出限为0.02~0.10μg/kg,定量限为0.10~0.30μg/kg。在5种基质中进行低中高3水平加标试验,其平均回收率为70.70%~105.00%,相对标准偏差为0.2%~11.1%(n=6)。该方法操作快捷、净化效果好、灵敏度高,适用于粮谷中酰胺类杀菌剂残留的定性定量分析。An improved QuEChERS purification method based on multi-walled carbon nanotubes(MWCNTs)was established,combined with liquid chromatography-tandem mass spectrometry for the determination of 14 amide pesticides in cereals.The samples were extracted by acetonitrile,cleaned up with anhydrous magnesium sulfate,PSA,MWCNTs and HC-C_(18).The 14 compounds were separated by symmetry C_(18) column,using positive ion scanning in multiple reaction monitoring(MRM),and finally quantified by the external standard method.The calibration curves for all analytes showed good linearity with correlation coefficients(r) of above 0.99 in the concentration range of 0.1-2.5 μg/L.The limits of detection(LOD) and the limits of quantification(LOQ) of the developed method were 0.02-0.1 and 0.1-0.3 μg/kg,respectively.The average recoveries in five different matrixes each spiked at low middle high three levels ranged from 70.7% to 105.0% with relative standard deviations(RSD) of 0.2%-11.1%(n=6).This method was fast to operate,showed good purification efficiency and sensitive.This method suitable for the determination of amide pesticides qualitative and quantitative analysis in cereals.

关 键 词：多壁碳纳米管 Qu ECh ERS 液相色谱-串联质谱法 粮谷 酰胺类杀菌剂 

分 类 号：TS207.53[轻工技术与工程—食品科学]