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
潘永波 1张妙宜 2万娜 1王彬 1潘灿平3
作者信息
- 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
- 折叠
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.
Abstract
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Key words
amino-functionalized multi-walled carbon nanotubes/QuEChERS/liquid chromatography-tandem mass spectrometry/tropical fruits/pesticide multi-residues引用本文复制引用
基金项目
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)
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-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)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据