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比较新型聚(3,4-亚乙基二氧噻吩)/氧化石墨烯复合涂层的固相微萃取中多环芳烃的直接进样、顶空和顶空冷纤维模式。

Comparison of direct, headspace and headspace cold fiber modes in solid phase microextraction of polycyclic aromatic hydrocarbons by a new coating based on poly(3,4-ethylenedioxythiophene)/graphene oxide composite.

机构信息

Faculty of Chemistry, Shahid Beheshti University, Tehran, Islamic Republic of Iran.

Faculty of Chemistry, Shahid Beheshti University, Tehran, Islamic Republic of Iran.

出版信息

J Chromatogr A. 2014 Jan 17;1325:23-30. doi: 10.1016/j.chroma.2013.11.056. Epub 2013 Dec 4.

Abstract

A novel nanocomposite coating made of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide was electrochemically prepared on gold wire. The prepared fiber was applied to the solid-phase microextraction (SPME) and gas chromatographic analysis of six polycyclic aromatic hydrocarbons (PAHs). Three modes of extraction i.e. direct immersion (DI), headspace (HS) and headspace cold fiber (HS-CF) in SPME were investigated. The results were compared under optimized conditions of each mode, considering the effects of the three most important parameters which are extraction temperature, extraction time and ionic strength. The comparison showed that HS-CF-SPME results in the best outcome for the extraction of PAHs from water samples. Under the optimized conditions of this mode, the calibration curves were linear within the range of 0.4-600μgL(-1) and the detection limits were between 0.05 and 0.13μgL(-1). The intra-day and inter-day relative standard deviations obtained at 10μgL(-1) (n=5), using a single fiber, were 4.1-6.8% and 4.8-8.4%, respectively. The fiber-to-fiber repeatabilities (n=4), expressed as the relative standard deviations (RSD%), were between 6.5% and 10.7% at a 10μgL(-1) concentration level. The method was successfully applied to the analysis of PAHs in seawater samples showing recoveries from 85% to 107%.

摘要

一种新型的聚(3,4-亚乙基二氧噻吩)(PEDOT)和氧化石墨烯纳米复合涂层通过电化学法在金线表面制备。所制备的纤维应用于固相微萃取(SPME)和气相色谱分析六种多环芳烃(PAHs)。研究了三种萃取模式,即直接浸入(DI)、顶空(HS)和顶空冷纤维(HS-CF)。在每种模式的优化条件下,考虑到萃取温度、萃取时间和离子强度三个最重要参数的影响,比较了结果。结果表明,HS-CF-SPME 对从水样中萃取 PAHs 效果最佳。在该模式的优化条件下,校准曲线在 0.4-600μgL(-1)范围内呈线性,检测限在 0.05-0.13μgL(-1)之间。在 10μgL(-1)(n=5)时,使用单个纤维获得的日内和日间相对标准偏差分别为 4.1-6.8%和 4.8-8.4%。在 10μgL(-1)浓度水平下,纤维间重复性(n=4)表示为相对标准偏差(RSD%)在 6.5%至 10.7%之间。该方法成功应用于海水样品中 PAHs 的分析,回收率为 85%至 107%。

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