色谱

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气相色谱-质谱法检测食品中残留的丙炔氟草胺

林黎,叶刚,谢丽琪,蓝芳,吴卫东,靳保辉

  

  1. Shenzhen Exit &Entry Inspection and Quarantine Bureau, Shenzhen 518067, China
  • 收稿日期:2007-08-22 修回日期:2007-10-22 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 叶刚

Determination of flumioxazin residue in foods using gas chromatography-mass spectrometry

LIN Li, YE Gang, XIE Liqi, LAN Fang, WU Weidong, JIN Baohui   

  1. Shenzhen Exit &Entry Inspection and Quarantine Bureau, Shenzhen 518067, China
  • Received:2007-08-22 Revised:2007-10-22 Online:2008-05-30 Published:1984-03-25
  • Contact: YE Gang

摘要:

建立了多种食品中丙炔氟草胺残留量的气相色谱-质谱检测方法。样品采用乙腈或乙酸乙酯提取,经旋转蒸发去除提取液后,用乙腈-甲苯(体积比为3∶1)溶解残渣,经氨基固相萃取柱净化,净化液由气相色谱-选择离子监测质谱测定,外标法定量。方法的线性范围为0.02~1.0 mg/L,多种食品基质中的平均回收率为79.4%~101%,相对标准偏差(RSD)为0.242%~7.15%(n=10),检测限均为0.01 mg/kg。该方法灵敏度高,选择性好,可作为多种食品中丙炔氟草胺残留量的常规检测方法。

关键词: 丙炔氟草胺, 固相萃取, 气相色谱-质谱法, 食品 , 选择离子监测

Abstract:

A method for the determination of flumioxazin residue in foods by gas chromatography-mass spectrometry (GC-MS) has been developed. The food sample was extracted with acetonitrile or ethyl acetate, concentrated in a rotary evaporator, then dissolved in acetonitrile-methyl benzene (3∶1, v/v) and purified with an NH2-solid phase extraction (SPE) column. The final extract was analyzed by gas chromatography-mass spectrometry with selected ion monitoring mode (GC-MS-SIM). External standard method was used for the quantification. The mean recoveries of flumioxazin spiked in foods were 79.4%-101%, and the relative standard deviations were 0.242%-7.15%(n=10). The detection limit for each was 0.01 mg/kg. This method has high sensitivity, veracity and is suitable for the determination of pesticide residues in foods.

Key words: flumioxazin, foods , gas chromatography-mass spectrometry (GC-MS), selected ion monitoring (SIM), solid phase extraction (SPE)