色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 654-659.DOI: 10.3724/SP.J.1123.2012.03039

• 研究论文 • 上一篇    下一篇

加速溶剂萃取-在线凝胶渗透色谱-气相色谱-质谱联用法快速测定蔬菜和水果中多农药残留

欧阳运富 唐宏兵 吴英 李贵英   

  1. 常州市疾病预防控制中心, 江苏 常州 213022
  • 收稿日期:2012-03-19 修回日期:2012-05-06 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 欧阳运富,硕士,副主任技师,主要从事色谱分析工作. Tel: (0519)86682659.
  • 基金资助:

    常州市自然科学基金项目(CS2008209).

Rapid determination of pesticide multiresidues in vegetables and fruits by accelerated solvent extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry

OUYANG Yunfu*, TANG Hongbing, WU Ying, LI Guiying   

  1. Changzhou Center for Disease Control and Prevention, Changzhou 213022, China
  • Received:2012-03-19 Revised:2012-05-06 Online:2012-07-28 Published:2012-07-19
  • Contact: Yun-Fu OUYANG

PDF

398

被引次数

46

摘要： 建立了加速溶剂萃取-在线凝胶渗透色谱-气相色谱-质谱联用(GPC-GC-MS)快速测定蔬菜、水果中代表性农药残留的检测方法。样品经二氯甲烷-丙酮(1:1, v/v)加速溶剂提取,活性炭柱-氨基柱串联净化,氮吹至干,残留物用环己烷-丙酮(7:3, v/v)溶解后经GPC-GC-MS系统以选择离子监测(SIM)模式测定。结果表明,22种农药在各自的线性范围内线性关系良好(相关系数不低于0.9981),检出限(以信噪比(S/N)为3计算)为0.3～1.8 μg/kg,定量限（S/N=10）为1~6 μg/kg。在2种基质(大白菜、苹果)中3个添加水平下的回收率为70.5%～107.5%,相对标准偏差为2.1%～8.7%。该方法提取效率高,定性定量准确、灵敏,可实现对蔬菜、水果中多农药残留的快速检测。

关键词: 多农药残留, 加速溶剂萃取, 凝胶渗透色谱, 气相色谱-质谱, 蔬菜, 水果

Abstract:  A novel method was developed for the rapid determination of 22 representative pesticide residues in vegetables and fruits based on accelerated solvent extraction (ASE) coupled with online gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS). The sample was extracted by accelerated solvent extraction with dichloromethane-acetone (1:1, v/v) and purified with a carbon/NH2 column, evaporated to dryness by nitrogen, then dissolved in cyclohexane-acetone (7:3, v/v), and finally identified and quantified by GPC-GC-MS system in selected ion monitoring (SIM) mode. The results showed that the linearities of the 22 pesticides were good in their linear ranges. The limits of detection (S/N=3) were 0.3~1.8 μg/kg. The limits of quantification (S/N=10) ranged from 1~6 μg/kg. The recoveries for all at three spiked levels in Chinese cabbages and apples ranged from 70.5% to 107.5% with the relative standard deviations (RSDs) of 2.1%~8.7%. The proposed method is accurate, sensitive and highly efficient in the extraction, and can be used for the quick determination of the pesticide multiresidues in vegetables and fruits.

Key words: fruits, gas chromatography-mass spectrometry (GC-MS) , gel permeation chromatography (GPC) , pesticide multiresidues, vegetables, accelerated solvent extraction (ASE)