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海绵状多孔氧化锰(II, III)作为涂层,用于溶剂辅助固相微萃取多环芳烃,然后进行气相色谱-质谱分析。

Sponge-like porous manganese(II, III) oxide as a coating for solvent-assisted solid-phase microextraction of polycyclic aromatic hydrocarbons followed by gas chromatography-mass spectrometry.

机构信息

Department of Chemistry, Isfahan University of Technology, Isfahan 8415683111, Iran.

Department of Chemistry, Isfahan University of Technology, Isfahan 8415683111, Iran.

出版信息

J Chromatogr A. 2022 Apr 26;1669:462947. doi: 10.1016/j.chroma.2022.462947. Epub 2022 Mar 9.

DOI:10.1016/j.chroma.2022.462947
PMID:35298937
Abstract

A nanostructure sponge-like porous manganese(II, III) oxide was synthesized and applied as a new fiber coating for solvent-assisted solid-phase microextraction. The synthesized material was characterized via Fourier-transform infrared spectroscopy, scanning electron microscopy, thermogravimetric analysis, X-ray diffraction, and N adsorption/desorption techniques. To investigate the extraction performance of the prepared material, direct immersion solid-phase microextraction followed by gas chromatography-mass spectrometry was used for the determination of the selected polycyclic aromatic hydrocarbons in wastewater samples. Three polycyclic aromatic hydrocarbons including 1-methylnaphthalene, anthracene, and pyrene were selected as model analytes. To maximize the sensitivity of the method, key experimental factors affecting the extraction efficiency of the analytes such as ionic strength, extraction solvent, stirring rate, extraction temperature and time, and desorption temperature and time were optimized. The applicability of the new coating material for the extraction of the selected analytes from wastewater samples was evaluated. Under the optimum conditions, detection limits between 0.7 and 1.5 ng L were obtained for the model analytes. The linear dynamic range was 5.0-3.0 × 10 ng L for all the analytes. Relative standard deviations were between 2 and 11%. In the case of real sample analysis, the extraction recoveries of the analytes were obtained in the range of 77-111%.

摘要

一种纳米结构的海绵状多孔锰(II, III)氧化物被合成,并被应用于作为一种新的纤维涂层,用于溶剂辅助固相微萃取。所合成的材料通过傅里叶变换红外光谱、扫描电子显微镜、热重分析、X 射线衍射和 N 吸附/解吸技术进行了表征。为了研究所制备材料的萃取性能,采用直接浸入固相微萃取,随后用气相色谱-质谱法测定废水中选择的多环芳烃。选择了三种多环芳烃,包括 1-甲基萘、蒽和芘作为模型分析物。为了最大限度地提高方法的灵敏度,优化了影响分析物萃取效率的关键实验因素,如离子强度、萃取溶剂、搅拌速度、萃取温度和时间以及解吸温度和时间。评估了新涂层材料对废水中选定分析物的萃取适用性。在最佳条件下,对模型分析物的检测限在 0.7 至 1.5 ng L 之间。所有分析物的线性动态范围为 5.0-3.0×10 ng L。相对标准偏差在 2-11%之间。在实际样品分析的情况下,获得了分析物的萃取回收率在 77-111%的范围内。

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