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固相萃取-气相色谱法测定饮用水中15种农药残留
Multi-residue determination method of pesticides in drinking water by solid-phase extraction followed by gas chromatography with electron capture detector
【摘要】 目的:建立同时检测饮用水中15种农药残留的固相萃取-气相色谱分析方法,所检测的农药包括5种有机磷、5种有机氯、5种拟除虫菊酯。方法:利用ENVI-C18固相萃取小柱提取水样中农药,小柱用甲醇和水活化,丙酮-正己烷(25:75,v/v)洗脱,浓缩后用GC-ECD测定。对水样前处理和色谱条件等进行了优化选择。结果:有机磷、拟除虫菊酯在0.05~1.0μg/ml,有机氯在0.01~0.2μg/ml浓度范围内有良好的线性,方法检出限为0.0021~0.032μg/L。样品平均加标回收率为70.2%~104.0%,精密度以平行样品的相对标准差(RSD)表示,为2.2%~13.0%。结论:本方法具有操作简单、准确、灵敏、重现性好、安全环保等优点,适用于饮用水中部分拟除虫菊酯、有机氯及有机磷的检测。
【Abstract】 Objective:A multiresidue method based on solid-phase extraction and gas chromatography with electron capture detector was developed for the simultaneous determination of 15 pesticides in drinking water.Methods:The extraction procedure was carried out in ENVI-C18 columns preconditioned with methanol and water.The subsequent elution of pesticides was performed with a mixture of acetone-hexane(25:75,v/v) prior to the determination by gas chromatography with electron capture detector.Results:Average recoveries for all the pesticides studied were higher than 70% and relative standard deviations were below 13% in the concentration range of 0.05~1.0 μg/ml for organophosphorous and pyrethroids,0.01~0.2 μg/ml for organochlorine.The method showed good linear ranges for all pesticides with correlation coefficients greater than 0.996.The detection limits achieved ranged from 0.0021~0.032 μg/L.Conclusion:This method is simple,rapid,sensitive,accurate and safe for determination of multiresidue of pesticides in drinking water.
【Key words】 Solid-phase extraction; Pesticide; Gas chromatography; Drinking water;
- 【文献出处】 中国卫生检验杂志 ,Chinese Journal of Health Laboratory Technology , 编辑部邮箱 ,2007年12期
- 【分类号】R123
- 【被引频次】28
- 【下载频次】449