超临界流体萃取法净化熟地中有机氯农药的研究

Study on removing organochlorine pesticide in Rehmanniae Preparata by supercritical fluid extraction

目的:去除熟地中残留的有机氯农药。方法:采用超临界CO2流体萃取法去除熟地中残留的有机氯农药,用毛细管气相色谱法测定除毒前后熟地中农药残留量,评价除毒率。用高效液相色谱法测定除毒前后熟地中梓醇及相关组分的变化,评价除毒后熟地药材的药用价值。结果:正交设计L9(34)选出最佳萃取条件为:压力15MPa,温度60℃,萃取时间30min,流速35kg.h-1。残留农药去除率达84.6%(RSD为3.7%)熟地中梓醇的相对含量101.1%(RSD为2.7%),相关组分含量没有显著性变化。结论:采用超临界CO2流体萃取法去除熟地中残留的有机氯农药,方法可行。

OBJECTIVE To remove residues of organochlorine pesticide in Rehmanniae Preparata. METHODS The organochlorine pesticide in Rehmanniae Preparata was extracted with supercritical CO2 fluid extrction, the residues of the organochlorine pesticide were determined before and after extraction by capillary gas chromatography, the removal rate was calculated, meanwhile the changes of the Catalpol and the related compositions were determined. RESULTS The best extraction condition selected by orthogonality design L9 （3^4） was pressure 15 MPa, temperature 60 ℃, the extracting time 30 min flownaling speed 35 kg·h^-1, the removal rate of the organochlorine pesticide 84. 6% （RSD = 3.7 % ）The relative contents of catalpol in Radix Rehmanniae Preparata was 101. 1 % ,and no remarkable change of the related compositions. CONCLUSION The approach is simple, convenient and stable and the removal rate is high and the contents of effective compositions have no noticeable change.