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基于三嗪的共价多孔有机聚合物用于高效液相色谱-二极管阵列检测前的多环芳烃在线管内固相微萃取。

Triazine-based covalent porous organic polymer for the online in-tube solid-phase microextraction of polycyclic aromatic hydrocarbons prior to high-performance liquid chromatography-diode array detection.

机构信息

Key Laboratory of Interfacial Reaction & Sensing Analysis in Universities of Shandong, School of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, PR China.

Key Laboratory of Interfacial Reaction & Sensing Analysis in Universities of Shandong, School of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, PR China.

出版信息

J Chromatogr A. 2021 Mar 29;1641:462004. doi: 10.1016/j.chroma.2021.462004. Epub 2021 Feb 18.

DOI:10.1016/j.chroma.2021.462004
PMID:33640808
Abstract

A triazine-based covalent organic porous polymer (COP) was synthesized from the monomers 1,3,5-triphenylbenzene and tricyanogen chloride via the Friedel-Crafts reaction and characterized in detail using Brunauer-Emmett-Teller analysis, X-ray photoelectron spectroscopy, elemental analysis, and scanning electron microscopy, which confirmed that the COP had a rough surface and suitable extraction site. It was then employed in in-tube solid-phase microextraction combined with a high-performance liquid chromatography-diode array detector. The COP adsorbent was evaluated with different types of analyte, including estrogens, polycyclic aromatic hydrocarbons (PAHs), and plasticizers. The COP produced its best performance with PAHs. In order to obtain the highest extraction efficiency for PAHs, the main influential factors were optimized. Furthermore, a sensitive analytical method was established with the limits of detection of 0.004-0.010 µg L, high enrichment factor of 1110-2763, and wide linear ranges (0.013-20.0 µg L, 0.016-20.0 µg L and 0.033-20.0 µg L). The relative standard deviation in intra-day and inter-day tests was also controlled to be within 0.3-3.1%. The proposed method was employed in the online detection of trace PAHs in real water samples, with satisfactory results obtained.

摘要

一种基于三嗪的共价有机多孔聚合物(COPs)是由单体 1,3,5-三苯基苯和三氰基氯通过傅-克反应合成的,并通过比表面积和孔径分布分析、X 射线光电子能谱分析、元素分析和扫描电子显微镜进行了详细的表征,证实 COP 具有粗糙的表面和合适的萃取位点。然后将其用于与高效液相色谱-二极管阵列检测器相结合的管内固相微萃取。评估了 COP 吸附剂对不同类型分析物的性能,包括雌激素、多环芳烃(PAHs)和增塑剂。COP 对 PAHs 的性能最佳。为了获得对 PAHs 的最高萃取效率,优化了主要影响因素。此外,建立了一种灵敏的分析方法,其检测限为 0.004-0.010 µg L,富集因子高达 1110-2763,线性范围较宽(0.013-20.0 µg L、0.016-20.0 µg L 和 0.033-20.0 µg L)。日内和日间测试的相对标准偏差也控制在 0.3-3.1%以内。该方法用于在线检测实际水样中的痕量 PAHs,结果令人满意。

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