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目的针对干蘑菇类样品基体特性,建立超声波二次辅助提取结合毛细管气相色谱测定其中有机氯农药六六六、滴滴涕含量的简便、快速的方法。方法干香菇、干黑木耳和干茶树菇样品分别打碎后以正己烷浸泡过夜,超声提取2次,提取液经过滤、氮吹进行浓缩,再以浓硫酸净化,离心吸取上清液后与标准溶液同批上机测定,以单点比较法定量。结果测定8种组分的方法检出限在3×10-5~2×10-4 mg/kg之间,3种样品加标回收率在79.6%~119.8%之间,精密度在1.4%~8.0%之间。结论该方法适用于干蘑菇类中有机氯农药六六六、滴滴涕的测定,且方法简便、准确,适合在实际检验工作中推广。
OBJECTIVE To establish a simple and rapid method for determining the content of hexachlorocyclohexane and DDT in organochlorine pesticides by secondary extraction by ultrasonic and capillary gas chromatography, Methods The samples of dried shiitake, dried black fungus and dried shiitake mushrooms were respectively smashed and soaked in n-hexane overnight. The mixture was extracted twice by ultrasonic. The extract was filtered, concentrated by nitrogen and purified by concentrated sulfuric acid. After centrifugation, The same batch of standard solution on the machine measured by single point comparison method. Results The detection limits of the eight components were between 3 × 10-5 and 2 × 10-4 mg / kg. The spiked recoveries of the three samples ranged from 79.6% to 119.8% with the precision of 1.4% ~ 8.0%. Conclusion The method is suitable for the determination of hexachlorocyclohexane and DDT in organochlorine pesticides in dried mushrooms. The method is simple, accurate and suitable for the promotion in practical testing.