分散液液微萃取-气相色谱联用检测果汁中有机磷类农药残留

Determination of Organophosphorous Pesticide Residues in Fruit Juices Samples Using Dispersive Liquid-liquid Microextraction Coupled with Gas Chromatography

如何检测果汁中的痕量农药残留是一个重要问题。今研究建立了分散液液微萃取（DLLME）结合气相色谱一火焰光度检测（GC—FPD）法检测果汁中8种有机磷农药残留新方法，并对影响液液微萃取效果的因素（如萃取剂和分散剂类型及用量、萃取时间和盐浓度等）进行了优化。在优化条件下，8种有机磷的富集倍数可达106～147；检出限（S／N=3）介于0．034-0．153μg·L。建立的新方法可用于多种果汁中农药多种残留检测，其平均加标回收率在74．7％～128．0％，相对标准偏差小于5．6％，完全满足果汁中有机磷类农药多种残留的检测要求。

How to determine trace multipesticide residues in fruit juices is an important problem. In this paper, a novel method was developed for the analysis of eight organophosphorus pesticide residues in fruit juice by using dispersive liquid-liquid microextraction（DLLME） coupled with gas chromatography-flame photometric detector （GC-FPD）. Parameters affecting the extraction performance, such as the species and volume of extraction and dispersive solvents, extraction time and salt concentration, were studied and optimized. Under the optimum extraction conditions, the enrichment factors range from 106 to 147 for eight kinds of organophosphorus pesticides, and the detection limits of the method are in the range of 0.034-0.153 gg.L-1. The developed method was successfully applied for the determination of multipesticide residues in various fruit juices, and the average spiked recoveries range from 74.7% to 128.0%, and relative standard deviations is less than 5.6%. Results show that the method proposed could completely meet the requirement for the determination of pesticide residues in fruit juices.