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聚吡咯/六方有序硅纳米复合材料作为新型固相微萃取纤维涂层。

Polypyrrole/hexagonally ordered silica nanocomposite as a novel fiber coating for solid-phase microextraction.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Iran.

出版信息

Anal Chim Acta. 2011 Oct 17;704(1-2):174-9. doi: 10.1016/j.aca.2011.07.045. Epub 2011 Aug 9.

Abstract

A highly porous fiber coated polypyrrole/hexagonally ordered silica (PPy/SBA15) materials were prepared for solid-phase microextraction (SPME). The PPy/SBA15 nanocomposite was synthesized by an in situ polymerization technique. The resulting material was characterized by the scanning electron microscopy, thermogravimetric analysis and differential thermal analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, desorption time and desorption temperature. In optimum conditions (extraction temperature 70°C, extraction time 20 min, ionic strength 20% (WV(-1)), stirring rate 500 rpm, desorption temperature 270°C, desorption time 5 min) the repeatability for one fiber (n=3), expressed as relative standard deviation (R.S.D. %), was between 5.0% and 9.3% for the tested compounds. The quantitation limit for the studied compounds were between 13.3 and 66.6 pg mL(-1). The life span and stability of the PPy/SBA15 fiber are good, and it can be used more than 50 times at 260°C without any significant change in sorption properties. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis.

摘要

一种高度多孔纤维涂覆聚吡咯/六方有序硅(PPy/SBA15)材料被用于固相微萃取(SPME)。PPy/SBA15 纳米复合材料通过原位聚合技术合成。所得材料通过扫描电子显微镜、热重分析和差示热分析进行了表征。将制备的纳米材料固定在不锈钢丝上,用于制备 SPME 纤维。纤维与气相色谱-质谱联用(GC-MS)结合,用于从水样中萃取一些多环芳烃(PAHs)。采用单因素优化策略,优化了萃取温度、萃取时间、离子强度、搅拌速度、解吸时间和解吸温度等重要萃取参数。在最佳条件下(萃取温度 70°C,萃取时间 20 分钟,离子强度 20%(WV(-1)),搅拌速度 500 rpm,解吸温度 270°C,解吸时间 5 分钟),对于测试的化合物,一根纤维(n=3)的重复性表示为相对标准偏差(R.S.D. %)在 5.0%到 9.3%之间。所研究化合物的定量限在 13.3 到 66.6 pg mL(-1)之间。PPy/SBA15 纤维的使用寿命和稳定性良好,在 260°C 下可以使用超过 50 次,而吸附性能没有明显变化。与传统分析方法相比,该方法具有操作简单、分析时间短、设备成本低、纤维热稳定性高、相对回收率高等优点。

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