GC-ECD法测定地龙药材中17种有机氯类农药残留  

Determination of 17 Organochlorine Pesticide Residue in Pheretima by GC-ECD

作　　者：李正刚 邵大志[1] 张亦萌 马彧[1] 马金刚[2] LI Zhenggang;SHAO Dazhi;ZHANG Yimeng;MA Yu;MA Jingang(Siping Institute for Food and Drug Control,Siping 136000,China;Siping Central People s Hospital,Siping 136000,China)

机构地区：[1]吉林省四平市食品药品检验所,吉林四平136000 [2]四平市中心人民医院,吉林四平136000

出　　处：《中国民族民间医药》2023年第18期45-48,共4页Chinese Journal of Ethnomedicine and Ethnopharmacy

基　　金：吉林省地方中药炮制规范项目(JLPZGF-2020-052)。

摘　　要：目的:采用气相色谱-电子捕获检测器(GC-ECD)检测不同产地的多批次地龙药材中17种有机氯类农药残留量。方法:样品经水、丙酮、适量氯化钠超声分散,二氯甲烷萃取,离心转移,有机相用无水硫酸钠脱水后减压浓缩至近干,正己烷溶解,硫酸溶液和水除去杂质,GC-ECD法测定。结果:在本实验条件下,17种农药组分能很好地分离检测,在测定范围0.76~100.30 ng/mL内线性关系良好,相关系数r均大于0.995,检出限在0.0015~0.0020 mg/kg之间,方法的重复性RSD均小于5.0%,加标回收率在81.2%~93.1%之间。结论:方法灵敏准确。收集的不同产地的10个批次样品中17种有机氯类农药均未检出,药材质量较好。Objective Determination of 17 organochlorine pesticide residues in different batches of Pheretima from different habitats by gas chromatography electron capture detector(GC-ECD).Methods The samples were dispersion with water,acetone and sodium chloride of appropriate amount by ultrasound;The pesticides were extracted with dichloromethane,centrifuged migrate.The organic phase was steamed to dry by reducing the pressure after dehydration with anhydrous sodium sulfate.Dissolveed by N-hexane,sulfuric acid solution and water to remove impurities,the pesticides were determined by GC-ECD.Results All the 17 pesticides showed good linearities in their reasonable rang(0.76-100.30 ng/mL),r^(2)>0.995,the LODs of each pesticide were all in the range of 0.0015-0.0020 mg/kg,the RSD of repeatability of the developed method was less than 5.0%,and the average recoveries of all the pesticides were in the range of 81.2%-93.1%.Conclusion The method is sensitive and accurate.17 organochlorine pesticides were not detected in 10 batches of samples collected from different habitats,and the quality of the medicinal materials was good.

关 键 词：气相色谱法 有机氯 农药残留 地龙 

分 类 号：R284.1[医药卫生—中药学]