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GC/MS 法快速分析鱼塘水中的硫丹

         

摘要

Objective Endosulfan has been often used to poison fish pond water in Jiangyin city. As the concentration of endosulfan in poisoned water is very low, it is revry difficult to detect endosulfan from water. In this paper, a new simple and rapid method for analysis of endosulfan in poisonedfish pond water was presented. Methods The dispersive liquid-liquid micro-extraction technique (DLLME) coupled with gas chromatography-ion trap mass spectrometric detection (GC-MS) was used to analyze endosulfan in samples of poisoned fish pond water. The disperser, containing extraction solvent, was rapidly injected into the sample solution with a syringe, making a cloudy solution formed. Because of the extraction solvent rapid diffusing into the sample solution and getting in touch with the analyte in the cloudy solution, the analyte was quickly transferred into the extraction solvent so that the extraction equilibrium could be achieved in a short time. After centrifuging, the fine particles of extraction solvent were precipitated in the bottom of the conical test tube and then were determined by GC-MS. Results Under the optimum conditions,the extraction rate of endosulfan in poisoned fish pond water was more than 90%, the limits of detection and the limits of quantitation were 0.005µg/mL and of 0.017µg/mL,respectively. The linear relation was quite good between 0.02µg/mL~0.20µg/mL. Conclusions The advantage of this new method is simple to operate, rapid, low cost, high recovery and accuracy. This method is suitable for casework.%目的:建立一种快速、高效、便捷、绿色的分析方法来分析鱼塘水中的硫丹。方法在该实验中采用分散液液微萃取的方法来提取鱼塘水中的硫丹,该方法是一个新型的预处理方法,首先将最合适的分散剂和萃取剂快速的注射到样品溶液中,随即形成了悬浊液。由于在悬浊液中萃取剂能迅速的分散到样品溶液中并与被分析物充分接触,被分析物能很快的从样品溶液中转移到萃取剂中完成萃取过程,经过离心后,沉积物直接用GC-MS 进行分析。同时还对本方法中分散剂和萃取剂种类、用量以及萃取时间等重要的实验参数进行考察优化。结果在优化的实验条件下,鱼塘水中硫丹的回收率基本能达到90%以上,检出限为0.005µg/mL,定量限为0.017µg/mL,在0.02~0.20µg/mL 的 z 范围内线性关系良好。结论该方法的准确度和精密度较好,操作简便、快捷、绿色环保,能够基本适合鱼塘投毒案件中硫丹的分析检测。

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