液-液萃取-气相色谱法测定水中9种有机氯农药
Determination of 9 Organochlorine Pesticides in Water Samples by Liquid-liquid Extraction-Gas Chromatography
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摘要: 采用正己烷液-液萃取法提取,气相色谱法-电子捕获检测器测定水中9种有机氯农药。优化了实验条件:添加两种替代物作为分析过程的质量监控; 使用浓硫酸磺化法净化去除杂质; 采用Rtx-5MS和Rtx-1701柱双柱定性,保证数据准确可靠。9种有机氯农药的方法检出限为0.0017~0.0079 μg/L,回收率为74.7%~105.1%,相对标准偏差(RSD,n=7)为4.2%~9.3%,9种农药在0.5~100 μg/L内与峰面积呈良好的线性关系。方法检出限低,准确度和精密度高,简便,适用于批量样品的分析。Abstract: Nine organochlorine pesticides were determined by gas chromatography with electron capture detector (ECD) after samples pre-treatment by liquid-liquid extraction with n-hexane and purified with concentrated sulfuric acid. The double capillary columns of Rtx-5MS and Rtx-1701 were used for identifying the target compounds. The experimental conditions were optimized and two surrogates were chosen for quality control. The detection limits of the method for 9 organochlorine pesticides were in the range of 0.0017~0.0079 μg/L with linear ranges of 0.5~100 μg/L. The recoveries were 74.7%~105.1% with the precision of 4.2%~9.3% RSD (n=7). The method provides the advantages of low detection limits, good accuracy and precision, simple operation and is suitable for routine analysis of organochlorine pesticides in water samples.