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在测定动物组织内有机氯农药滴滴涕,666残留量的工作中碰到的一个问题,是如何去掉提取液中的脂肪等杂质。过去一般多用液-液分配、酸性硅藻土、柱层等方法进行净化,但这些方法多费时费事,操作繁琐。最近,我们测定鸡体内(鸡肉、鸡肝和脂肪)滴滴涕,666含量的工作中, 为加快分析速度,摸索了使用浓硫酸净化的方法,效果很好,简便易行。净化之样品可供薄层、气相色谱仪测定,无杂质干扰,回收率也较高。三只鸡九个重复α-666回收率达90％以上。pp’-滴滴涕回收率达100％。(在鲤鱼提取液内加药用浓硫酸净化看对666、滴滴涕几个异构体的回收情况如下:回收率α-666 74％;β-666 107％;γ-666 94.6％;pp’-滴滴涕103％;op’-滴滴涕 95％;pp’-滴滴涕109％)。测定动物体内酸稳定性农药的残留量,均可用浓硫酸净化。现以鸡肉为样品,将此法介绍,供参考。
One of the problems encountered in the determination of residues of organochlorine pesticides DDT, 666 in animal tissues is how to remove impurities such as fat from the extract. In the past the general use of liquid - liquid distribution, acidic diatomaceous earth, column and other methods for purification, but these methods are more time-consuming and complicated operation. Recently, in order to speed up the analysis of DDT and 666 in chickens, chicken livers and fats, we explored the method of using concentrated sulfuric acid to purify, which is effective and easy to operate. Purified samples for thin layer, gas chromatograph determination, no impurities, the recovery rate is also higher. Three chickens nine repeat α-666 recovery rate of more than 90%. pp’- DDT recovery rate of 100%. (In the carp extract with medicinal concentrated sulfuric acid purification see 666, DDT several isomers of the recovery as follows: Recovery of α-666 74%; β-666 107%; γ-666 94.6%; pp’- DDT 103%; op’-DDT 95%; pp’-DDT 109%). Determining the amount of acid-stable pesticide residues in animals can be purified with concentrated sulfuric acid. Now chicken as a sample, this method is introduced for reference.