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

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[J]. 分析化学, 2017, 45(11): 1711-1718. doi: 10.11895/j.issn.0253-3820.171160 shu

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[J]. Chinese Journal of Analytical Chemistry, 2017, 45(11): 1711-1718. doi: 10.11895/j.issn.0253-3820.171160 shu

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

武汉理工大学化学化工与生命科学学院化学系, 武汉 430070
基金项目:
本文系国家自然科学基金项目（No.21476177）资助

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 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:

English

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

Department of Chemistry, School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, China
Received Date: 09 August 2017
Revised Date: 18 September 2017
Fund Project:
This work was supported by the National Natural Science Foundation of China (No. 21476177).

Abstract: A method for the determination of 15 kinds of nitroaromatics in aqueous samples was developed by dispersive liquid-liquid microextraction and gas chromatography with electron capture detection. A high-density extractant applied in electron capture detector was screened out. The chromatographic conditions, types and dosages of extractants, types and dosages of dispersants, extraction time and the extraction temperature were optimized. The results showed that DB-35 capillary column had the best separation performance for the 15 kinds of nitroaromatics. The nitroaromatics could be separated within 22 min using programmed temperature control as follows:holding at an initial temperature of 80℃ and then heating to 180℃ at a ramping rate of 5℃/min. For the extraction of 15 kinds of nitroaromatics from 5 mL of aqueous sample, the extraction equilibrium could be reached within 30 s with a high extraction recovery of over 90% when using 100 μL of chlorobenzene as extracting solvent and 400 μL of methanol as disperser solvent. In addition, the enrichment factor could approach a high value of 45.0-48.8. The sediment collected by centrifugation was injected and analyzed by gas chromatography with electron capture detector. The limits of quantification of the developed method were 0.03-0.15 μg/L (S/N=10). The linear range was from 0.20 μg/L to 50.0 μg/L, while the correlation coefficients (R²) were more than 0.998. At the spiked level of 0.200 μg/L, the relative standard deviations of this method were 3.3%-8.9%, the relative recoveries ranged from 86.0% to 103.5%. At higher spiked level, the relative standard deviations were less than 5%, and the relative recoveries ranged from 94.5% to 101.5%.

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

English

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

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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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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