乳制品中16种有机氯农残的的气相色谱测定方法

Detection of 16 Pesticide Residue of Chlorine Pesticides in Dairy Products by GC Method

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。

Currently, the most common methods to detect pesticide residues of organic chlorine in dairy products are gas chromatograph（GC） and gas chromatography tandem mass spectrometry（GC-MS/MS）, which take a long time for sample pretreatment, and need much consumptive material. In this paper, we adopt acetone and n-hexane to process samples, and pass through the Florsil Solid Phase Extract Column（SPE cartridges） for GC method, which is simple, quick and helpful to discount the cost. A good clean-up result was obtained and no interference for target peaks. A good separation was shown for 16 kinds of pesticide residues of organic chlorine by the improved instrumental conditions, especially for several isomers like endosulfan and chlordane. The reliability and accuracy of this method are verified by analyzing the chromatographic peak performance parameters and the recovery of standard addition of the target compounds. For this method, the recovery rate is 87.4 to 103.4%, good repeatability and low detection limit were observed, and the cost was reduced, whcih is suitable for fast analysis of organic chlorine pesticide residues in milk products for the labs without mass spectrometry.