Ouyang Yunfu, Tang Hongbing, Wu Ying, Li Guiying
Changzhou Center for Disease Control and Prevention, Changzhou 213022, China.
Se Pu. 2012 Jul;30(7):654-9. doi: 10.3724/sp.j.1123.2012.03039.
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 microg/kg. The limits of quantification (S/N = 10) ranged from 1-6 microg/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.
基于加速溶剂萃取（ASE）结合在线凝胶渗透色谱-气相色谱-质谱联用（GPC-GC-MS）技术，开发了一种快速测定蔬菜和水果中22种代表性农药残留的新方法。样品用二氯甲烷-丙酮（1:1，v/v）通过加速溶剂萃取法提取，并用碳/NH2柱净化，经氮气吹干后，溶解于环己烷-丙酮（7:3，v/v）中，最后在选择离子监测（SIM）模式下通过GPC-GC-MS系统进行定性和定量分析。结果表明，22种农药在其线性范围内线性良好。检测限（S/N = 3）为0.3-1.8 μg/kg。定量限（S/N = 10）为1-6 μg/kg。在大白菜和苹果中三个加标水平下，所有农药的回收率在70.5%至107.5%之间，相对标准偏差（RSDs）为2.1%-8.7%。该方法在提取过程中准确、灵敏且高效，可用于快速测定蔬菜和水果中的多种农药残留。
