分散液液微萃取-气相色谱法快速测定水中15种硝基苯类物质

发布时间：2018-05-26 03:51

本文选题：气相色谱 + 分散液液微萃取　；参考：《分析化学》2017年11期

【摘要】：建立了分散液液微萃取-气相色谱电子捕获检测器测定水中15种硝基苯类物质的方法。筛选出了具有高密度且能够适用于电子捕获检测器的萃取剂。优化了色谱条件,对萃取剂种类及用量、分散剂种类及用量、萃取时间、萃取温度等条件进行了优化。DB-35毛细管柱对15种硝基苯类物质具有最好的分离效果。使用程序升温,初始80℃保持2 min,以5℃/min速率升温至180℃,可以在22 min内完成分离。以100μL氯苯作为萃取剂、400μL甲醇作为分散剂,对5.00 m L水样在室温下进行萃取,仅需30 s即可达到萃取平衡,15种目标物的萃取率均可达到90%以上,富集倍数达到45.0~48.8。离心分离,取下层沉积相进行气相色谱测定,使用电子捕获检测器检测,方法的定量限为0.03~0.15μg/L,线性范围为0.20~50.0μg/L,相关系数不低于0.998。方法的相对标准偏差在3.3%~8.9%之间,加标回收率在86.0%~103.5%之间。
[Abstract]:A method for the determination of 15 nitrobenzene compounds in water by dispersive liquid liquid microextraction and gas chromatography electron capture detector was established. The extraction agent with high density and suitable for electronic capture detector was selected. The conditions of chromatography, the type and dosage of extractant, the species and dosage of dispersant, the extraction time, the extraction temperature and other conditions were optimized. The optimized.DB-35 capillary column has the best separation effect for 15 nitrobenzene compounds. Using the programmed temperature, the initial 80 C is maintained at 2 min and the temperature of 5 C /min is heated to 180 C, and the separation can be completed in 22 min. 100 mu L chlorobenzene is used as the extractant and 400 micron methanol is used as the dispersant, and the 5 m L water samples are extracted at room temperature only. The extraction balance can be achieved by 30 s, the extraction rate of the 15 targets can reach more than 90%, the enrichment multiple reaches 45.0~48.8. centrifuge separation, the lower layer sedimentary facies is determined by gas chromatography, and the quantitative limit of the method is 0.03~0.15 mu g/L, the linear enclosure is 0.20~50.0 u g/L, and the correlation coefficient is not lower than the 0.998. method. The relative standard deviation is between 3.3%~8.9%, and the recovery of standard addition is between 86.0%~103.5%.
【作者单位】：武汉理工大学化学化工与生命科学学院化学系;
【基金】：国家自然科学基金项目(No.21476177)资助~~
【分类号】：O657.71;X832

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