加速溶剂萃取-气相色谱法检测土壤中14种有机氯农药方法

Analysis of 14 Organochlorine Pesticides in Soil by Accelerated Solvent Extraction/Gas Chromatography

建立了加速溶剂萃取-气相色谱检测土壤中14种有机氯农药(OCPs)的方法。对影响OCPs回收率的主要因素进行优化,得出优化条件:1次静态萃取循环,萃取温度90℃,静态萃取时间3 min,冲洗量30%,氮气吹扫时间40 s,正己烷/丙酮(1∶1,V/V)为萃取液。在优化条件下,加标水平为10、100?g/L时,平均加标回收率为86.6%～120%、88.1%～120%,相对标准偏差(n=7)均小于10%,方法检出限(t值法)为1.03～2.64?g/L。

A analytical method for the determination of 14 organochlorine pesticides （OCPs） in soil using accelerate solvent extraction followed by gas chromatography analysis was developed. The main potential influence parameters which affected the recoveries of OCPs were investigated. Finally, 1 static extraction cycle, 90℃ of extraction temperature, 3 min of static extraction time, 30% of rinse volume, 40 s of nitrogen purge time and mixture of hexane and acetone （1∶1, V/V） as extraction solvent were determined. Under the optimized conditions, the average spiked recoveries for the samples products at the spiked levels of 10 and 100 μg/L were in the range of 86.6%-120% and 88.1%-120%, meanwhile the relative standard deviations （n=7） less than 10%, moreover the method detection limits were characterized as 1.03-2.64 μg/L.