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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。
Objective To establish a method for the determination of pentachlorophenol and 2,4-dichloro-6-nitrophenol in urine by gas chromatography. Methods Blank urine was used to add pentachlorophenol and 2,4-dichloro-6-nitrophenol standard and the internal standard 2,4-dichlorophenol. After acetic anhydride derivatization, the samples were detected by gas chromatography The extraction methods, derivatization conditions were investigated. Results Gas chromatography analysis showed that pentachlorophenol and 2,4-dichloro-6-nitrophenol in urine could be effectively separated without any interference and the peak shape was better. At pH 2, cyclohexane was the optimal extraction condition. The derivatization conditions are as follows: using 10 μL of acetic anhydride and adding 10 μL of anhydrous pyridine, and reacting at 60 ° C. for 30 min. Conclusion The method of gas chromatography for the determination of pentachlorophenol and 2,4-dichloro-6-nitrophenol in urine is simple and accurate. It can be used in practical treatment.