GC-ECD法测定蜂房药材中17种有机氯类农药残留

Determination of 17 organochlorine pesticide residues in medical products derived from the Nidus Vespae by gas chromatography-electron capture detector analysis

目的建立气相色谱-电子捕获检测检测器法(GC-ECD)检测蜂房中17种有机氯类农药残留。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,采用GC-ECD法测定。结果在实验条件下,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,r均大于0.995,检出限在0.0011~0.0018 mg/kg之间,方法的重复性相对标准偏差均小于3.3%,加标回收率在90.7%~98.1%。结论该方法适合测定蜂房中17种有机氯类农药残留。

Objective To develop a gas chromatography-electron capture detector(GC-ECD)method to determine 17 organochlorine pesticide residues in medical products derived from the Nidus Vespae.Methods The samples were dispersed in mixtures of water,acetone and sodium chloride of appropriate amount by ultrasound waves,in which pesticide residues were extracted with dichloromethane,centrifuged and transferred to evaporators.The organic phase was evaporated to nearly dryness by reducing the pressure after dehydration with anhydrous sodium sulfate.After being dissolved by n-hexane and treated with sulfuric acid solution and water to remove impurities,the pesticide residues were determined by GC-ECD.Results Under the experimental conditions,17 pesticides showed good linearities in their reasonable range(0.76-100.30 ng/ml),with a r value>0.995,and the limit of detection of each pesticide was in the range of 0.0011-0.0018 mg/kg,the relative standard deviation of repeatability of the developed method was less than 3.3%,and the average spiked recoveries of all the pesticides were in the range of 90.7%-98.1%.Conclusion The method is appropriate for the determination of 17 organochlorine pesticide residues in medical products derived from the Nidus Vespae.