SPE-GC-ECD法测定中成药中20种有机氯类农药残留量

SPE-GC-ECD determination of 20 organochlorine pesticides residue in Chinese medicinal products

目的:建立中成药中20种有机氯农药残留量的测定方法。方法:采用正己烷作为提取溶剂,经弗罗里硅土小柱净化,选用电子捕获检测器(ECD)进行气相色谱测定。结果:20种有机氯农药在0.4～500μg·L^(-1)范围内呈良好的线性关系;检测限在0.04～2.62μg·L^(-1)之间,定量限在0.12～7.94μg·L^(-1)之间;低(5μg·L^(-1))、中(50μgL^(-1))、高(100μg·L^(-1))3个水平的添加回收试验的回收率(n=18)为72.2～125.3%,各回收率的RSD在3.2%～20.7%之间,符合残留量测定的有关要求。结论:方法简便、准确可靠,重复性较好,可作为中成药中有机氯农药残留的检验方法。

Objective ： To establish a new method for determination of the residue of 20 kinds of organochlorine pesticides（OCPs） in Chinese medicinal products . Methods：The samples were extracted by n- hexane,the extraction were cleaned up through florisil SPE column and determined by GC with μ -ECD. Results：There were good linear relationships over the range of 0. 4- 500μg·L^-1for 20 OCPs. The limits of detection and quantification ranged from 0.04 - 2. 62μg·L^-1 and 0. 12 - 7.94μg·L^-1 , respectively. Average recoveries of 20 OCPs added at the three levels of 5,50 and 100μg·L^-1 were 72.2% - 125.3% , with RSD in the range of 3.2% -20. 7%. Conclusion ： The established method was simple and reliable, with good reproducibility and can be used for determination of OCPs residue in Chinese medicinal products.