色谱

色谱

• 研究论文 • 上一篇    下一篇

凝胶渗透色谱净化-气相色谱/串联质谱分析蘑菇中的36种农药残留

于胜良1,2,杨桂朋1,付萌2

  

  1. 1.Key Laboratory of Marine Chemistry Theory and Technology, Ministry of Education, Ocean Chemistry,
    Ocean University of China, Qingdao 266003, China; 2.Sino Analytica Laboratory of
    Pesticide Residue Analysis of Agricultural Products, Qingdao 266012, China
  • 收稿日期:2007-01-11 修回日期:2007-03-01 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 于胜良

Determination of 36 Pesticide Residues in Mushroom by Gel
Permeation Chromatography and Gas Chromatography-
Tandem Mass Spectrometry

YU Shengliang1,2, YANG Guipeng1, FU Meng2   

  1. 1.Key Laboratory of Marine Chemistry Theory and Technology, Ministry of Education, Ocean Chemistry,
    Ocean University of China, Qingdao 266003, China; 2.Sino Analytica Laboratory of
    Pesticide Residue Analysis of Agricultural Products, Qingdao 266012, China
  • Received:2007-01-11 Revised:2007-03-01 Online:2007-07-30 Published:1985-06-25

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摘要：

建立了用凝胶渗透色谱净化-气相色谱/串联质谱分析蘑菇中36种农药残留的方法。蘑菇中的待测农药组分在30 ℃条件下用乙酸乙酯提取,高速匀浆后通过凝胶渗透色谱净化;选用填料为中性多孔的聚苯乙烯二乙烯基苯微球体的S-X3玻璃柱(22 g,19 cm×2 cm)作为凝胶渗透色谱净化柱,流动相为乙酸乙酯-环己烷(体积比为1∶1)溶液,流速5 mL/min;收集第7~15 min流出的液体用气相色谱-三重四极杆串联质谱仪测定。在0.01~1.0 mg/L的质量浓度范围内,各种农药标准溶液的线性相关系数均大于0.99。在样品中添加36种农药(添加水平为0.01,0.05,0.10 mg/kg)的混合标准溶液,平均回收率为72.6%~117.1%,相对标准偏差为2.0%~10.8%(n=5),最低检出限为 0.1~0.7 μg/kg,最低定量限为 0.2~2 μg/kg。

关键词: 残留检测, 蘑菇 , 凝胶渗透色谱, 农药, 气相色谱/串联质谱

Abstract:

A gel permeation chromatographic method was developed for the extraction of 36 pesticides from mushroom prior to gas chromatography with a triple quadrupole mass spectrometric determination. The extraction was based on homogenization with ethyl acetate using a high speed homogenizer. A gel permeation chromatographic clean-up process with ethyl acetate-cyclohexane (1∶1, v/v) as mobile phase was applied to the extracts to separate the low-molecular mass pesticides from the high molecular mass compounds in the mushroom. The 7-15 min eluate fraction was collected for subsequent analysis. The target compounds were quantified in the final extract by gas chromatography using a triple quadrupole mass spectrometer with multiple reaction monitoring (MRM). In the linear range (0.01-1.0 mg/L) of each pesticide, the correlation coefficient was higher than 0.99.The average recoveries (spiked at the levels of 0.01, 0.05, 0.10 mg/kg) were from 72.6% to 117.1% with the relative standard deviations from 2.0% to 10.8%(n=5). The limits of detection (LOD) for these pesticides were from0.1 to 0.7 μg/kg and the limits of quantification (LOQ) were from 0.2 to 2 μg/kg.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), mushroom , pesticides, residue determination, gel permeation chromatography (GPC)