氨基化-多壁碳纳米管QuEChERS-液相色谱-串联质谱法测定热带水果中110种农药及其代谢物残留量  

Determination of 110 pesticide and their metabolites residues in tropical fruits using QuEChERS with amino-functionalized multi-walled carbon nanotube and liquid chromatography-tandem mass spectrometry

作　　者：潘永波 张妙宜 万娜 王彬 潘灿平[3] PAN Yongbo;ZHANG Miaoyi;WAN Na;WANG Bin;PAN Canping(Institute of Food Testing,Hainan Academy of Inspection and Testing,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation,Haikou 570314,China;Institute of Tropical Bioscience and Biotechnology,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China;College of Science,China Agricultural University,Beijing 100193,China)

机构地区：[1]海南省检验检测研究院食品检验检测中心国家市场监管重点实验室(热带果蔬质量与安全),海口570314 [2]中国热带农业科学院热带生物技术研究所,海口571101 [3]中国农业大学理学院,北京100193

出　　处：《农药学学报》2024年第1期189-202,共14页Chinese Journal of Pesticide Science

基　　金：国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(ZZ-2022006,ZZ-2023024);国家市场监管重点实验室(热带果蔬质量与安全)基础应用及重点研究课题资助(KF2023012)。

摘　　要：建立基于氨基化-多壁碳纳米管(amino-functionalized multi-walled carbon nanotubes,NH2-MWCNTs)改进的QuEChERS净化方法,结合液相色谱-串联质谱(LC-MS/MS)测定3种热带水果中110种农药及其代谢物残留量。样品经乙腈提取,采用欧洲标准(EN.15662)萃取缓冲体系QuEChERS盐包提取,NH2-MWCNTs改良的分散固相萃取(d-SPE)净化管净化,多反应监测模式(MRM)分析,基质匹配标准曲线外标法定量。结果表明:在0.002~0.2 mg/L范围内110种农药及其代谢物具有良好的线性关系,决定系数(R2)均高于0.9902,定量限(LOQ)为0.005~0.05 mg/kg,添加回收率为61%~120%,相对标准偏差(RSD)为0.30%~15%(n=6)。该方法净化效果好,能在短时间内可靠地分析样品。灵敏度、正确度、精密度均满足日常检测定性、定量需求,适用于荔枝、龙眼和香蕉等热带水果中农药多残留的快速检测。Combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS),an improved QuEChERS method was established based on amino-functionalized multi-walled carbon nanotubes(NH2-MWCNTs)for the determination of 110 pesticides and their metabolites in three tropical fruits.The samples were extracted by acetonitrile,salted out by QuEChERS salt package with European standard(EN.15662)buffer system,purified by dispersed solid phase extraction(d-SPE)with NH2-MWCNTs sorbents,analyzed at multi-reaction monitoring mode(MRM),and quantified using external standard method with matrix-matched calibration curves.The results showed good linearity(R2>0.9902)for the 110 pesticides and their metabolites in the range of 0.002-0.2 mg/L.The limits of quantification(LOQs)ranged from 0.005 to 0.05 mg/kg.The recoveries were 61%~120%,and the relative standard deviations(RSDs)were 0.30%to 15%(n=6).This method exhibits excellent purification performance and takes less time for the sample analysis.The validation results met the requirements for qualitative and quantitative analysis of pesticides with high sensitivity,accuracy,and precision.It is suitable for rapid detection of multiple pesticide residues in tropical fruits such as litchi,longan and banana.

关 键 词：氨基化-多壁碳纳米管 QUECHERS 液相色谱-串联质谱 热带水果 农药多残留 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]