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用于微固相萃取的核壳结构电纺聚对苯二甲酸丁二醇酯/聚吡咯中空纳米纤维

Core-shell electrospun polybutylene terephthalate/polypyrrole hollow nanofibers for micro-solid phase extraction.

作者信息

Bagheri Habib, Rezvani Omid, Banihashemi Solmaz

机构信息

Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.

Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.

出版信息

J Chromatogr A. 2016 Feb 19;1434:19-28. doi: 10.1016/j.chroma.2015.12.082. Epub 2016 Jan 12.

Abstract

In the present work, a new micro-solid phase extraction (μ-SPE) sorbent as an extracting medium based on core-shell nanofibers was synthesized by electrospinning. The core-shell nanofibers of polyvinylpyrrolidone-Polybutylene terephthalate/polypyrrole (PVP-PBT/PPy) were electrospun and subsequently, modified hollow nanofibers were prepared by removing the central PVP moiety. Moreover, conventional PBT/PPy was also prepared for the comparison purposes. The homogeneity and the porous surface structure of the core-shell nanofibers were confirmed by scanning electron microscopy (SEM). The applicability of the fabricated nanofibers-coating was examined by immersed μ-SPE of some selected triazine herbicides from aqueous samples and wheat grains. Subsequently, the extracted analytes were transferred into a gas chromatography (GC) after solvent desorption. Influencing parameters on the morphology of nanofiber such as elctrospinning parameters and the weight ratio of components were optimized. In addition, effects of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength, sample pH, desorption temperature, and desorption time were investigated and optimized. Eventually, the developed method was validated by gas chromatography-mass spectrometry (GC-MS). At the optimum conditions, the relative standard deviation values for real water samples spiked with the selected triazines at 1 ng mL(-1) were 4-8% (n=3) and the limits of detection for the studied compounds were between 50 and 90 ng L(-1). The calibration curves for the selected triazines were in the range of 0.3-500 ng mL(-1) and regression coefficients (R(2)) were between 0.9985 and 0.9996.

摘要

在本研究中,通过静电纺丝合成了一种新型的微固相萃取(μ-SPE)吸附剂,该吸附剂以核壳纳米纤维作为萃取介质。静电纺丝制备了聚乙烯吡咯烷酮-聚对苯二甲酸丁二醇酯/聚吡咯(PVP-PBT/PPy)核壳纳米纤维,随后通过去除中心的PVP部分制备了改性中空纳米纤维。此外,还制备了传统的PBT/PPy用于对比。通过扫描电子显微镜(SEM)确认了核壳纳米纤维的均匀性和多孔表面结构。通过从水样和小麦籽粒中对一些选定的三嗪类除草剂进行浸入式μ-SPE,考察了所制备的纳米纤维涂层的适用性。随后,溶剂解吸后将萃取的分析物转移至气相色谱(GC)中。优化了诸如静电纺丝参数和组分重量比等影响纳米纤维形态的参数。此外,研究并优化了影响萃取效率的不同参数,包括萃取温度、萃取时间、离子强度、样品pH值、解吸温度和解吸时间。最终,通过气相色谱-质谱联用(GC-MS)对所建立的方法进行了验证。在最佳条件下,向实际水样中添加1 ng mL⁻¹选定三嗪类物质时,相对标准偏差值为4-8%(n=3),所研究化合物的检测限在50至90 ng L⁻¹之间。选定三嗪类物质的校准曲线范围为0.3-500 ng mL⁻¹,回归系数(R²)在0.9985至0.9996之间。

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