中药材中农药残留提取方法比较研究

摘要

Objective To compare the effects of accelerated solvent extraction (ASE), ultrasonic extraction (USE) and soxhlet extraction (SE), by extraction and determination of pesticide residues in Chinese herbal medicines. Methods Pesticide residues of Chinese herbal medicines were extracted by accelerated solvent extraction, ultrasonic extraction and soxhlet extraction, then the extract were cleaned up by sulfonation treatment, alumina neutral-florisil column and gel permeation chromatography (GPC). The extract was separated by HP-5 capillary column and detected by electron-capture detector. Results Extraction efficiency of USE was significantly lower than that of ASE and SE, there was no significant difference between ASE and SE. Pairwise comparison of the recoveries of three purification methods showed no significant difference. Conclusion The extraction efficiency of three methods was ASE>SE>USE. The extraction method should be selected according to the requirement.%目的：比较加速溶剂萃取、超声提取和索氏提取法3种常用提取方法对中药材中残留农药的提取差异。方法用加速溶剂萃取、超声提取和索氏提取分别对含有已知农药残留的中药材进行残留农药提取,经浓硫酸磺化、弗罗里硅土柱净化和凝胶渗透色谱3种净化方法,采用HP-5毛细管色谱柱分离样品,气相色谱-电子捕获检测器测定其农药残留的含量,外标法定量。结果超声提取的提取率显著低于索式提取、加速溶剂萃取(P＜0.05),加速溶剂萃取与索式提取的提取率差异无统计学意义(P＞0.05),3种净化方法回收率两两比较差异无统计学意义(P＞0.05)。结论加速溶剂萃取的提取率最高,其次为索氏提取,超声提取最低。检测者应根据需要选取不同的提取方法。