色谱

色谱 ›› 2011, Vol. 29 ›› Issue (02): 115-119.DOI: 10.3724/SP.J.1123.2011.00115

• 研究论文 • 上一篇    下一篇

分散液-液微萃取与气相色谱-质谱联用分析环境水样中痕量的2,4-二硝基甲苯和磷酸三(2-氯乙基)酯

熊珺1*, 谢思龙2, 赖毅东1   

  1. 1. 广东省东莞市质量监督检测中心, 广东 东莞 523808; 2. 华南理工大学轻工与食品学院, 广东 广州 510641
  • 收稿日期:2010-11-01 修回日期:2010-12-16 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 熊珺,博士,从事痕量化合物检测技术的研究
  • 基金资助:

    广东省质量技术监督局科技项目(No. 2008SJ027).

Simultaneous determination of 2,4-dinitrotoluene and tris(2-chloroethyl)ester in environmental waters by dispersive liquid-liquid microextraction combined with gas chromatography-mass spectrometry

XIONG Jun1*, XIE Silong2, LAI Yidong1   

  1. 1. Guangdong Dongguan Quality Supervision Testing Center, Dongguan 523808, China; 2. College of Light Industry and Food Sciences, South China University of Technology, Guangzhou 510641, China
  • Received:2010-11-01 Revised:2010-12-16 Online:2011-02-28 Published:2007-03-25

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705

被引次数

9

摘要： 建立了分散液-液微萃取与气相色谱-质谱联用同时测定环境水样中痕量2,4-二硝基甲苯和磷酸三(2-氯乙基)酯的新方法。对影响萃取效率的因素进行了详细的考察和优化,确定采用的最佳萃取条件为: 将0.8 mL乙醇和60 μL氯仿的混合溶液快速注入5.0 mL的样品溶液中,振动混匀120 s后,离心分离,吸取沉积在试管底部的氯仿相直接进样分析。该方法对磷酸三(2-氯乙基)酯和2,4-二硝基甲苯的检出限(信噪比为3)分别为0.01和0.04 μg/L,富集倍数分别为96.6和127.5;两种物质的线性范围达3到4个数量级;日内和日间测定的相对标准偏差(RSDs, n=6)分别为8.6%～11.5%和8.9%～12.0%。将该方法用于环境水样中2,4-二硝基甲苯和磷酸三(2-氯乙基)酯的分析,其加标回收率为102.1%～110.9%。方法具有操作简单、方便快速、灵敏度高、无交叉污染和环境友好等优点。

关键词: 2,4-二硝基甲苯, 分散液-液微萃取, 环境水样, 磷酸三(2-氯乙基)酯, 气相色谱-质谱

Abstract: A method based on dispersive liquid-liquid microextraction-gas chromatography-mass spectrometry (DLLME-GC-MS) was developed for the simultaneous determination of trace 2,4-dinitrotoluene (2,4-DNT) and tris(2-chloroethyl)ester (TCEP) in environmental water samples. The types of extraction solvent, dispersive solvent, extraction time and ionic strength were investigated and optimized to obtain the best extraction efficiency for the target analytes. The analysis performance evaluation and the real sample analysis were performed as follows: 0.8 mL of ethanol as dispersive solvent and 60 μL of chloroform as extraction solvent were rapidly added into 5.0 mL of the aqueous solution, and the solution was vibrated about 120 s and centrifuged. Then the sediment phase to be analyzed was directly injected into a GC-MS. Under the optimized conditions, the limits of detection (LODs, S/N=3) for the target analytes were 0.01 μg/L and 0.04 μg/L with the enrichment factors (EFs) of 96.6 and 127.5. The real environmental water samples were analyzed and the recoveries of 102.1%~110.9% were obtained. The method is simple, fast, efficient and inexpensive.

Key words: 2, 4-dinitrotoluene, environmental water samples, gas chromatography-mass spectrometry, tris (2-chloroethyl) ester, Dispersive liquid-liquid microextraction