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尿中五氯酚和2,4-二氯-6-硝基苯酚气相色谱分析
Determination of pentachlorophenol and 2,4-dichloro-6-nitrophenol in urine by gas chromatography
【摘要】 目的建立利用气相色谱分析检测尿中五氯酚和2,4-二氯-6-硝基苯酚的方法。方法取空白尿液添加五氯酚和2,4-二氯-6-硝基苯酚标准品及内标2,4-二氯苯酚,经乙酸酐衍生化后,采用气相色谱法进行检测,并对提取方法、衍生化条件等进行考察。结果经气相色谱分析,尿中五氯酚和2,4-二氯-6-硝基苯酚可得到有效分离,无杂质干扰且峰形较好。在pH值为2条件下,以环己烷作为萃取溶剂为最佳萃取条件。衍生化优选条件为使用10μL乙酸酐并加入10μL无水吡啶,60℃反应30min。结论采用气相色谱法检测尿中五氯酚和2,4-二氯-6-硝基苯酚,方法简单、结果准确,可在实际办案中应用。
【Abstract】 Objective A method for the detection of pentachlorophenol and 2,4-dichloro-6-nitrophenol in urine by gas chromatography was developed.Methods After derivatized with acetic anhydride,pentachlorophenol,2,4-dichloro-6-nitrophenol and 2,4-dichlorophenol in blank urine were determined accurately by gas chromatography.The effects of several important factors,such as the methods of extraction and conditions of derivative were investigated.Results By using gas chromatography,pentachlorophenol and 2,4-dichloro-6-nitrophenol in urine can be separated effectively without impurity interference.The optimal conditions for extraction were using cyclohexane as solvent in pH2.The excellent conditions for derivatization were 60℃,30min,10μL acetic anhydride and 10μL pyridine.Conclusion The method is simple and effective.It can be used for the casework.
【Key words】 forensic toxicological analysis; acetylation; pentachlorophenol; 2,4-dichloro-6-nitrophenol;
- 【文献出处】 中国法医学杂志 ,Chinese Journal of Forensic Medicine , 编辑部邮箱 ,2011年03期
- 【分类号】D919
- 【被引频次】5
- 【下载频次】252