色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱/质谱法分析水果和蔬菜中残留的嘧菌酯

薄海波   

  1. Qinghai Entry-Exit Inspection and Quarantine Bureau, Xining 810000, China
  • 收稿日期:2007-04-18 修回日期:2007-08-02 出版日期:2007-11-30 发布日期:1984-12-25
  • 通讯作者: 薄海波

Determination of Azoxystrobin Residues in Fruits and Vegetables by Gas Chromatography/Mass Spectrometry with Solid-Phase Extraction

BO Haibo   

  1. Qinghai Entry-Exit Inspection and Quarantine Bureau, Xining 810000, China
  • Received:2007-04-18 Revised:2007-08-02 Online:2007-11-30 Published:1984-12-25
  • Contact: BO Haibo

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摘要：

建立了多种水果和蔬菜中嘧菌酯残留的气相色谱/质谱分析方法。首先用乙酸乙酯-环己烷(体积比为1∶1)对样品中的嘧菌酯进行超声波提取,经硅胶固相萃取小柱对样品提取液进行净化、富集,采用气相色谱/质谱法以选择离子监测模式(m/z 344,372,388,403定性,m/z 344定量)进行检测。实验结果表明,嘧菌酯在0.01～1.0 mg/kg浓度范围内呈线性,其相关系数r>0.99。在低、中、高3个添加水平,嘧菌酯的回收率为85.2%～98.2%,相对标准偏差为5.8%～21.5%。方法的检测限不大于0.01 mg/kg,定量限不大于0.05 mg/kg。

关键词: 残留分析, 固相萃取, 嘧菌酯, 气相色谱-质谱法, 蔬菜 , 水果

Abstract:

A method was developed for the determination of azoxystrobin residues in fruits and vegetables by gas chromatography/mass spectrometry (GC/MS). Azoxystrobin residues were extracted with ethyl acetate-cyclohexane (1∶1, v/v) by ultrasonication and then they were cleaned up on a silica solid-phase extraction (SPE) column to obtain an extract suitable for analysis by GC/MS in the selective ion monitoring (SIM) mode (the selected ion: m/z 344, 372, 388 and 403). The calibration curves were linear between area and concentration of azoxystrobin from 0.01 to 1.0 mg/kg with the correlation coefficient greater than 0.99. The average recoveries from spiked fruit and vegetable matrixes at three concentrations of 0.01, 0.1, 1.0 mg/kg ranged from 85.2% to 98.2% with relative standard deviation less than 21.5%. The limit of detection was 0.01 mg/kg and the limit of quantity was 0.05 mg/kg in fruit and vegetable matrixes, respectively.

Key words: azoxystrobin, fruits, residue analysis, solid-phase extraction, vegetables , gas chromatography/mass spectrometry