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QuEChERS-高效液相色谱-串联质谱法测定丙炔氟草胺在食品和环境中的残留及土壤中的消解动态

程功 刘娜 田宏哲 朱赫 纪明山

农药学学报2018,Vol.20Issue(1):75-82,8.
农药学学报2018,Vol.20Issue(1):75-82,8.DOI:10.16801/j.issn.1008-7303.2018.0016

QuEChERS-高效液相色谱-串联质谱法测定丙炔氟草胺在食品和环境中的残留及土壤中的消解动态

Residue analysis of flumioxazin in food and environment by modified QuEChERS method using high performance liquid chromatography- tandem mass spectrometry and the dissipation dynamics in soil

程功 1刘娜 1田宏哲 1朱赫 1纪明山1

作者信息

  • 1. 沈阳农业大学植物保护学院,沈阳 110866
  • 折叠

摘要

Abstract

A rapid, simple, sensitive and effective analytical method for the determination of flumioxazin in food (apple, grape, wheat, soybean, cabbage, and orange), soil and water based on a QuEChERS procedure was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with acetonitrile and cleaned-up by dSPE with C18, GCB, PSA mixed with MgSO4 as sorbent in different matrices. The samples were detected by using an Eclipse Plus C18 column connected to an electrospray ionization source in positive mode (ESI+), monitoring(MRM) mode. The matrix-matched external standard calibration curves were used forquantitative analysis. The results showed that the linearity of flumioxazin in the range of 0.01-5 mg/kg, with determination coefficients higher than 0.9976. The intra-day average recoveries ranged from 82%-104% in eight matrices at three levels (0.01, 0.1 and 1 mg/kg) and the relative standard deviation (RSD) ranged from 1.1%-7.8% (n = 5). The inter-day average recoveries ranged from 77%-109% in eight matrices at three levels (0.01, 0.1 and 1 mg/kg) and the RSD ranged from 0.1%-9.2% (n = 15). The LOQs ranged from 0.0003-0.0032 mg/kg, which were lower than the maximum residue limits (MRLs) of flumioxazin established by America, the European Union, Japan, and China. It can detect the residues of flumioxazin in food and environmental samples. Based on this method, the dissipation dynamics of flumioxazin in the field soil was characterized, which provided a theoretical basis for the risk assessment of food safety and environment pollution.

关键词

QuEChERS/高效液相色谱-串联质谱/丙炔氟草胺/食品/土壤//残留/消解

Key words

QuEChERS/high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)/flumioxazin/food/soil/water/residue/dissipation

分类

农业科技

引用本文复制引用

程功,刘娜,田宏哲,朱赫,纪明山..QuEChERS-高效液相色谱-串联质谱法测定丙炔氟草胺在食品和环境中的残留及土壤中的消解动态[J].农药学学报,2018,20(1):75-82,8.

农药学学报

OA北大核心CSCDCSTPCD

1008-7303

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