超声波-固相萃取测定木香中七种有机氯农药残留前处理方法研究.doc

摘要：本实验应用超声波及固相萃取技术，以体积比4:1的正己烷:甲醇混合溶液作为溶剂对云木香中的α、β、γ、和δ-六六六及2,4′-DDT、4,4′-DDT和七氯等7种有机氯农残的提取净化前处理方法进行了初步的系统研究，研究了不同超声时间对提取效率的影响、不同比例的二氯甲烷:石油醚洗脱剂对净化效率的影响并对比了弗罗里硅土小柱与C18小柱的净化效果差异，获得了较优的提取净化前处理工艺条件为:超声30分钟；使用弗罗里硅土小柱；洗脱剂为体积比3:7的二氯甲烷:石油醚混合溶液。论文实验数据通过标准加入法，利用岛津GC-2010气相色谱ECD检测器定量分析并计算回收率获得所得数据响应较好，相关系数均大于0.99，初步建立了超声波-固相萃取测定木香中七种有机氯农药残留的较优前处理方法。优化条件下测出木香中的δ-六六六及2,4′-DDT，而其余5种未检出。　

关键词：超声波；固相萃取；净化；有机氯农药；木香

ABSTRACT：This experiment used ultrasound affected solid-phase microextraction technique, with the volume of positive than 4:1 by cyclohexane as solvent methanol mixed solution to cloud the alpha, beta, woody gamma, and delta - HCH and 2 ,4'- DDT, 4,4'-DDT and heptachlor and so on - seven kinds of organochlorine pesticides residues pre-treatment methods of extraction purification conducts a preliminary study of the system of ultrasonic time different influence of extraction efficiency, different proportions of methylene chloride: petroleum ether elution agents on the influence of purification efficiency and compared Florisil Small column and C18 Small column purifying effect difference, obtained a optimal extraction purification process before conditions for: ultrasound 30 minutes; Use Florisil Small column; Elution agents for the volume ratio of 3:7 methylene chloride: petroleum ether mixture. Papers experimental data through the standard addition method, using the Shimadzu- 2010 gas chromatography (GC) ECD detector quantitative analysis and calculation,obtained data recovery rate get good response, correlation coefficient are larger than 0.99 , ultrasonic - solid phase microextraction determination of pre-treatment methods of organochlorine pesticides residues than seven optimal treatments.Under the optimized conditions , getting wood-aromatic delta - HCH and 2,4′-DDT, but the rest of the five was not detected .

Keywords:ultrasonic; solid-phase microextraction; organochlorine pesticides; wood-aromatic;  purification