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易于合成具有球形结构的共轭微孔聚合物,用于固相萃取苯脲类除草剂。

Facile synthesis of conjugated microporous polymer with spherical structure for solid phase extraction of phenyl urea herbicides.

机构信息

Department of Chemistry, College of Science, Hebei Agricultural University, Baoding 071001, China; College of Food Science and Technology, Hebei Agricultural University, Baoding 071001, China.

Department of Chemistry, College of Science, Hebei Agricultural University, Baoding 071001, China.

出版信息

J Chromatogr A. 2020 Jul 5;1622:461131. doi: 10.1016/j.chroma.2020.461131. Epub 2020 Apr 29.

Abstract

A carbazolic conjugated microporous polymer (designated as CZ-CMP) was successfully synthesized through Scholl reaction of carbazole with 1, 3, 5-triphenylbenzene. The CZ-CMP was characterized by FT-IR spectrum, X-ray diffraction, nitrogen sorption isotherms, and scanning electron microscopy. The characterization results showed that the CZ-CMP had a spherical structure with high surface area and good microporosity. Its adsorption performance was investigated by applying it as an adsorbent for the solid phase extraction (SPE) of phenyl urea herbicides (PUHs) (metoxuron, chlortoluron, isoproturon, monolinuron and buturon) from tea drinks samples prior to high performance liquid chromatographic detection. The CZ-CMP displayed high extraction efficiency for the PUHs, and the primary factors affecting the SPE efficiency including the type and volume of the eluent, sample solution pH, sample loading rate and sample volume were optimized. Under the optimized conditions, a good linear response for the analytes was observed in the range of 0.10-80.0 ng mL with correlation coefficients (r) from 0.9937 to 0.9997. The limits of detection were measured to be in the range of 0.02-0.30 ng mL and the limits of quantitation were in the range of 0.06-0.9 ng mL. The developed method was successfully applied for the determination of the five PUHs in four different kinds of drinks with the method recoveries between 83.7% and 118% and the relative standard deviations between 1.0% and 10%. Besides, the application potential of the CZ-CMP was evaluated by using it to extract different types of the organic compounds including some phthalate eaters (PAEs), chlorophenol (CPs), nitroimidazoles and polycyclic aromatic hydrocarbons (PAHs). The results indicated that the CZ-CMP had strong adsorption ability for the compounds with more hydrogen bonding sites and moderate hydrophobicity.

摘要

一种咔唑稠合微孔聚合物(命名为 CZ-CMP)通过咔唑与 1,3,5-三苯基苯的 Scholl 反应成功合成。通过傅里叶变换红外光谱、X 射线衍射、氮气吸附等温线和扫描电子显微镜对 CZ-CMP 进行了表征。表征结果表明,CZ-CMP 具有球形结构,具有高比表面积和良好的微孔性。将其用作固相萃取(SPE)的吸附剂,用于从茶饮料样品中提取苯脲类除草剂(PUHs)(甲氧隆、氯隆、异丙隆、单隆和丁隆),然后进行高效液相色谱检测,以研究其吸附性能。CZ-CMP 对 PUHs 具有高萃取效率,影响 SPE 效率的主要因素包括洗脱剂的类型和体积、样品溶液 pH 值、样品加载速率和样品体积进行了优化。在优化条件下,分析物在 0.10-80.0ng mL 范围内呈现良好的线性响应,相关系数(r)为 0.9937-0.9997。检测限测量值在 0.02-0.30ng mL 范围内,定量限在 0.06-0.9ng mL 范围内。该方法成功应用于四种不同饮料中五种 PUHs 的测定,方法回收率在 83.7%-118%之间,相对标准偏差在 1.0%-10%之间。此外,通过使用 CZ-CMP 提取不同类型的有机化合物,包括一些邻苯二甲酸酯(PAEs)、氯酚(CPs)、硝基咪唑和多环芳烃(PAHs),评估了 CZ-CMP 的应用潜力。结果表明,CZ-CMP 对具有更多氢键供体和适度疏水性的化合物具有较强的吸附能力。

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