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引用本文:   杜小弟, 李俊升, 郭丽萍, 雷家珩. 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. 分析化学, 2017, 45(11): 1711-1718. doi:  10.11895/j.issn.0253-3820.171160 [复制]

Citation:   DU Xiao-Di, LI Jun-Sheng, GUO Li-Ping, LEI Jia-Heng. Determination of 15 Kinds of Nitroaromatics in Aqueous Samples Using Dispersive Liquid-Liquid Microextraction and Gas Chromatography with Electron Capture Detection. Chinese Journal of Analytical Chemistry, 2017, 45(11): 1711-1718. doi: 10.11895/j.issn.0253-3820.171160 [复制]

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

通讯作者:  雷家珩, yhx2000@263.net

收稿日期: 2017-08-09

接受日期: 2017-09-18

出版日期: 2017-11-20

基金项目: 本文系国家自然科学基金项目(No.21476177)资助

Determination of 15 Kinds of Nitroaromatics in Aqueous Samples Using Dispersive Liquid-Liquid Microextraction and Gas Chromatography with Electron Capture Detection

Corresponding author:  LEI Jia-Heng, yhx2000@263.net

Received Date:  2017-08-09

Accepted Date:  2017-09-18

Published Date:  2017-11-20

Fund Project:  This work was supported by the National Natural Science Foundation of China (No. 21476177)

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 mL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。

关键词:   气相色谱, 分散液液微萃取, 硝基苯类, 饮用水
Key words:   Gas chromatography, Dispersive liquid-liquid microextraction, Nitroaromatics, Drinking water
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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

杜小弟, 李俊升, 郭丽萍, 雷家珩

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