GC-ECD法测定人参归脾丸中17种有机氯类农药残留

Determination of 17 organochlorine pesticide residues in Renshen Guipi Pills by GC-ECD

目的 建立气相色谱-电子捕获检测法(GC-ECD)同时测定人参归脾丸中17种有机氯农药残留量。方法 人参归脾丸样品经水、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,采用GC-ECD法测定样品中17种有机氯类农药残留。结果 17种有机氯类农药在测定范围0.76~100.30 ng/ml内线性关系良好,线性相关系数(r)均大于0.995,检出限(LOD)为0.001 1~0.001 8 mg/kg,平均回收率为73.6%~110.1%。结论 该方法灵敏度高,准确可靠,可用来测定人参归脾丸中17种有机氯类农药残留量。

Objective To establish a method of simultaneous determination 17 organochlorine pesticide residues in Rensh⁃en Guipi pills by gas chromatography electron capture detection(GC-ECD).Methods The samples were dispersion with water,acetone and sodium chloride of appropriate amount by ultrasound;The pesticides were extracted with dichlorometh⁃ane,centrifuged migrate.The organic phase was steamed to dry by reducing the pressure after dehydration with anhydrous so⁃dium sulfate.Dissolveed by N-hexane,sulfuric acid solution and water to remove impurities,the pesticides were determined by GC-ECD.Results All the 17organochlorine pesticides showed good linearities in the reasonable rang of 0.76 to 100.30 ng/ml with the linear collection coefficients(r)greater than 0.995.The LODs of each pesticide were all in the range of 0.0011-0.0018 mg/kg,and the average recoveries of all the pesticides were in the range of 73.6%-110.1%.Conclusion This method is highly sensitive,accurate and reliable and can be used to determine 17 organochlorine pesticide residues in Renshen Guipi pills.