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目前测定乳制品中有机氯农药残留多采用气相色谱方法或气质联用法,样品前处理比较费时、繁琐,处理所用的耗材成本也比较高。本文采用丙酮和正己烷提取样品,用Florisil固相萃取小柱净化,去除杂质干扰的效果好,测定乳及乳制品中16种有机氯农药残留,目标峰没有干扰。通过改进气相色谱仪器条件,使16种有机氯农残的目标峰得到较好的分离,尤其是硫丹和氯丹几种异构体得到了比较好的分离。通过对目标化合物色谱峰性能参数和加标回收率的的分析,验证了本方法的可靠性和准确性。本方法使用价格比较低廉的气相色谱仪,分析乳制品中有机氯农药残留,回收率达到87.4~103.4%,测定重复性好,检出限较低,准确可靠,非常适合没有质谱分析仪的实验室快速分析乳制品中有机氯农药残留。
At present, the determination of organochlorine pesticide residues in dairy products using gas chromatography or GC-MS method is more time-consuming and cumbersome than the sample preparation, and the cost of consumables used in the treatment is also relatively high. In this paper, acetone and n-hexane samples were extracted with Florisil solid phase extraction cartridge purification, removal of impurities interference effect, determination of 16 kinds of organochlorine pesticides residues in milk and dairy products, the target peak without interference. By improving the gas chromatograph conditions, the target peaks of 16 kinds of organochlorine pesticides were well separated, especially the isomers of endosulfan and chlordane were well separated. The reliability and accuracy of the method were verified by analyzing the performance parameters of the target compounds and the spike recoveries. The method uses a relatively inexpensive gas chromatograph to analyze residues of organochlorine pesticides in dairy products, and the recovery rate reaches 87.4-103.4%. The method has the advantages of good repeatability, lower detection limit, accurate and reliable, and is very suitable for experiments without a mass spectrometer Rapid Analysis of Organochlorine Pesticide Residues in Dairy Products.