中药栓剂中有机氯农药残留量测定方法的探索研究(Ⅱ)

Methodological Study of Determining Organochlorine Pesticides Residue in Suppositories of Chinese Medicinal Materials(Ⅱ)

目的选择合适的固相萃取方法,对前述的中药栓剂(以脂溶性基质为主)供试液进一步净化处理,使适用于中药栓剂(以脂溶性基质为主)中的20种有机氯类农药残留量测定。方法选用不同的固相萃取柱及固相萃取洗脱条件,对中药"化痔栓"供试液进一步净化处理,用GC—ECD法进行定量测定,并用20种有机氯农药混合标准品对其进行加标回收试验。结果待测定的各有机氯农药标准品回收率基本达到农药残留分析的要求。结论样品供试液经GPC柱洗脱后,再经弗罗里硅土小柱净化处理,可进一步去除杂质,达到准确定量的目的。

Objective To develop a suitable solid -phase extraction （SPE） method for the further purification of the test solution in suppositories of Chinese medicinal materials which are made of lipid soluble bases, and to detect the residues of 20 kinds of organochlorine pesticides（OCPs）. Methods Different kinds of SPE columns were selected and several elution solvents were used for the purification of the sample of herbal medicine of Huazhi Shuan, and then the residue contents of OCPs were determined by GC - ECD method. Twenty kinds of OCPs were added into the samples and the efficacy of the methods were evaluated by the obtained recoveries. Results The recoveries of the 20 kinds of OCPs being detected were basically comply with the requirements for the analysis of pestiside residues. Conclusion After the tested solution is obtained from GPC column and is further purified through florisil SPE column, the impurity can De removed and the high accuracy of the quantitative analysis of the compounds can be achieved.