色谱

色谱 ›› 2015, Vol. 33 ›› Issue (5): 455-460.DOI: 10.3724/SP.J.1123.2015.01025

• 特别策划：新型分离材料专栏 • 上一篇    下一篇

溶胶-凝胶杂化整体柱修饰及在多环芳烃检测中的应用

杨然存1,2, 张少文2, 孙雨安1   

  1. 1. 郑州轻工业学院, 河南 郑州 450000;
    2. 洛阳理工学院, 河南 洛阳 471023
  • 收稿日期:2015-01-21 出版日期:2015-05-08 发布日期:2015-04-23
  • 通讯作者: 张少文, 孙雨安
  • 基金资助:

    河南省科技发展计划项目(122102310333,1223041346);河南省教育厅基础前沿项目(13A150793).

Modification of sol-gel hybrid monolith and its application in determination of polycyclic aromatic hydrocarbons

YANG Rancun1,2, ZHANG Shaowen2, SUN Yu'an1   

  1. 1. Zhengzhou University of Light Industry, Zhengzhou 450000, China;
    2. Luoyang Institute of Science and Technology, Luoyang 471023, China
  • Received:2015-01-21 Online:2015-05-08 Published:2015-04-23

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128

被引次数

1

摘要：

利用点击反应对含叠氮基的溶胶-凝胶整体柱进行了表面修饰,制备了C6-硅胶杂化整体萃取柱。实验以多环芳烃为分析对象,考察了制备和修饰条件对萃取效率的影响,在优化的条件下,新制备的整体柱对萘、菲、芘和苯并[a]芘的萃取富集倍数分别达到95.9、114.2、103.2和57.8。萃取实验的日内和日间精密度(RSD)分别小于5.5%(n=8)和7.3%(n=10)。建立的管内固相微萃取-高效液相色谱检测16种常见多环芳烃方法的检出限(S/N=3)达到0.08~3.72 μg/L,定量限(S/N=10)达到0.26~12.40 μg/L。土壤中多环芳烃分析的加标回收率为82.4%~110.6%, RSD为2.6%~7.9%(n=3)。与美国国家环境保护局检测土壤中多环芳烃的方法比较,结果一致,准确性高。实验表明,该方法萃取效率高,灵敏可靠,操作简便,重现性好,可满足土壤等样品中痕量多环芳烃检测的要求。

关键词: 点击反应, 多环芳烃, 高效液相色谱, 管内固相微萃取, 硅胶杂化整体柱

Abstract:

A C6-silica hybrid monolithic column was prepared by click reaction with capillary silica monolith. Firstly, an azide-functionalized silica monolithic column was synthesized via sol-gel reaction with tetramethoxysilane (TMOS) and 3-azidopropyltrimethoxysilane (N3PTMS). Then 1-hexyne was covalently immobilized on the capillary monolith by the "azide-alkyne" click reaction to form C6-silica hybrid monolithic column. As an extraction media of polycyclic aromatic hydrocarbons (PAHs), the conditions for the preparation and modification of the monolith were carefully investigated according to the extraction efficiency. The enrichment factors for typical PAHs: naphthalene, phenanthrene, pyrene and benzo[a]pyrene finally reached 95.9, 114.2, 103.2 and 57.8, respectively. The relative standard deviations (RSDs) for the extraction were lower than 5.5% (intra-day, n=8) and 7.3% (inter-day, n=10). Based on the in-tube solid phase microextraction (in-tube SPME), a new determination method for 16 PAHs was developed with high performance liquid chromatography (HPLC). The limits of detection (LODs, S/N=3) were 0.08-3.72 μg/L and the limits of quantification (LOQs, S/N=10) were 0.26-12.40 μg/L for the PAHs. The spiked recoveries for the PAHs in soil samples were between 82.4% and 110.6% with the RSDs (n=3) of 2.6%-7.9%. Comparison with the method of United States Environmental Protection Agency (U. S. EPA) for the PAHs determination in soil samples, the results showed good accuracy and high consistency. And the high extraction efficiency with high sensitivity and convenience was also demonstrated in the applications of the new approach.

Key words: click reaction, high performance liquid chromatography (HPLC), in-tube solid phase microextraction (SPME), polycyclic aromatic hydrocarbons (PAHs), silica hybrid monolith

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