改良QuEChERS方法结合超高效液相色谱串联质谱测定茶树组织中的双丙环虫酯和代谢物M440I007

doi:10.13305/j.cnki.jts.2024.03.010

摘要/Abstract

摘要： 双丙环虫酯是一种新型生物源杀虫剂,2023年在我国登记用于茶树中茶小绿叶蝉的防治。建立了改良QuEChERS法结合超高效液相色谱-串联质谱法（UPLC-MS/MS）测定茶树组织中双丙环虫酯及其代谢物M440I007的分析方法。茶树根、茎、叶经水和乙腈提取,N-丙基乙二胺（PSA）、羟基化多壁碳纳米管（MWCNT-OH）和石墨化炭黑（GCB）净化,目标物用UPLC-MS/MS多反应监测模式（MRM）测定,基质匹配标准曲线外标法定量。在0.002~5.000 mg·L^-1范围内,两种化合物的线性关系良好,决定系数（R²）>0.999 5。在0.005~2.000 mg·kg^-1的添加水平下,两种化合物的回收率为78.3%~106.0%,相对标准偏差（RSD）≤12.85%,方法的定量限（LOQ）和检出限（LOD）分别为0.005 mg·kg^-1和0.002 mg·kg^-1。采用该方法,测得盆栽施药处理土壤培养7 d的茶苗组织中双丙环虫酯的分布为根（0.102 mg·kg^-1）>茎（0.078 mg·kg^-1）>叶（0.007 mg·kg^-1）,其转运因子TF_root-stem和TF_stem-leaf均小于1,代谢物M440I007的残留水平均在定量限以下。本研究建立的方法成本低、准确度和灵敏度高,可为进一步研究双丙环虫酯和M440I007在茶树中的吸收传导行为提供技术基础。

关键词: 茶树, 农残, 双丙环虫酯, M440I007, 检测方法

Abstract: Afidopyropen, a novel biorational insecticide, was registered in China in 2023 for the control of tea leafhoppers in tea plantation. In this study, an analytical method was developed for the determination of afidopyropen and its metabolite M440I007 in tea tissues by a modified QuEChERS method combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Roots, stems and leaves of tea plants were extracted by water and acetonitrile, and purified with primary secondary amine (PSA), hydroxylated multi-walled carbon nanotubes (MWCNT-OH) and graphitized carbon black (GCB). The target compounds were determined by UPLC-MS/MS in multiple reaction monitoring (MRM) mode, and quantified by external standard method with matrix-matched standard curve. Both targets display excellent linearity (R²>0.999 5) in the range of 0.002-5.000 mg·L^-1. The recoveries of both compounds at the spiked levels of 0.005-2.000 mg·kg^-1 ranged from 78.3% to 106.0% with the relative standard deviations (RSD) ≤ 12.85%. The limits of quantification (LOQs) and detection (LODs) of the method were 0.005 mg·kg^-1and 0.002 mg·kg^-1, respectively. The developed method was applied to detect afidopyrofen and M440I007 in tea seedling tissues cultured in soil treated with afidopyropen in a pot experiment for 7 days. The results show that the distribution of afidopyropen in the tissues was roots (0.102 mg·kg^-1) > stems (0.078 mg·kg^-1) > leaves (0.007 mg·kg^-1). The translocation factors, TF_root-stem and TF_stem-leaf, were both less than 1, and the residue levels of the metabolite M440I007 were below the LOQ. The method established in this study is low-cost, accurate and sensitive, which can serve as a technical basis for further research on the uptake and transport behaviors of afidopyropen and M440I007 in tea plants.

Key words: tea plant, pesticide residues, afidopyropen, M440I007, detection method

中图分类号:

S571.1
S482

秦钰洁, 郭明明, 陈永晶, 周利. 改良QuEChERS方法结合超高效液相色谱串联质谱测定茶树组织中的双丙环虫酯和代谢物M440I007[J]. 茶叶科学, 2024, 44(3): 515-525. doi: 10.13305/j.cnki.jts.2024.03.010.

QIN Yujie, GUO Mingming, CHEN Yongjing, ZHOU Li. Determination of Afidopyropen and Metabolite M440I007 in Tea Tissues by Modified QuEChERS Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Tea Science, 2024, 44(3): 515-525. doi: 10.13305/j.cnki.jts.2024.03.010.

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