College of Science, Hebei Agricultural University, Baoding 071001, Hebei, China.
College of Landscape and Travel, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2018 May 25;1551:1-9. doi: 10.1016/j.chroma.2018.03.053. Epub 2018 Mar 28.
A covalent organic framework named TpAzo was successfully fabricated by a simple and environmentally friendly mechanochemical grinding method based on the Schiff base aldehyde-amine condensation reaction between 1,3,5-triformylphloroglucinol (Tp) and 4,4'-azodianiline (Azo), with p-toluene sulphonic acid as a molecular organizer. The TpAzo was characterized by scanning electron microscopy, transmission electron microscopy, powder X-ray diffraction, nitrogen adsorption-desorption isotherms, and thermogravimetric analysis. The TpAzo possessed a sheet-like morphology, rich porosity and high thermal stability. The extraction performance of the TpAzo was investigated by using it as the solid phase extraction adsorbent for the extraction of benzoylurea insecticides (BUs) from juice, tomato and white radish samples prior to high performance liquid chromatographic analysis. Under the optimal conditions, a good linearity for the BUs existed in the range of 1.0-160.0 ng mL for juice sample and 0.5-80.0 ng g for tomato and white radish samples with the correlation coefficients of 0.9956-0.9999. The limits of detection for the analytes were 0.1-0.2 ng mL for juice sample and 0.05-0.1 ng g for tomato and white radish samples. The method recoveries for the analytes fell in the range of 84.1%-108.6%. The adsorption mechanism of the TpAzo was investigated by using it to extract different types of organic compounds, including phthalates, phenylurea herbicides and carbamate insecticides. The results showed that the π-stacking and hydrophobic interactions between the TpAzo and the analytes played an important role for the adsorption.
一种名为 TpAzo 的共价有机骨架通过基于席夫碱醛-胺缩合反应的简单环保机械化学研磨方法成功制备，该反应是在 1,3,5-均苯三甲醛（Tp）和 4,4'-偶氮二苯胺（Azo）之间进行的，对甲苯磺酸作为分子组织者。TpAzo 通过扫描电子显微镜、透射电子显微镜、粉末 X 射线衍射、氮气吸附-解吸等温线和热重分析进行了表征。TpAzo 具有片状形态、丰富的孔隙率和高热稳定性。TpAzo 被用作固相萃取吸附剂，用于从果汁、番茄和白萝卜样品中萃取苯甲酰脲类杀虫剂（BUs），然后进行高效液相色谱分析，研究了其萃取性能。在最佳条件下，BUs 在果汁样品的 1.0-160.0ngmL 和番茄和白萝卜样品的 0.5-80.0ngg 范围内具有良好的线性关系，相关系数为 0.9956-0.9999。分析物的检出限为 0.1-0.2ngmL 果汁样品和 0.05-0.1ngg 番茄和白萝卜样品。分析物的回收率在 84.1%-108.6%范围内。通过用 TpAzo 萃取不同类型的有机化合物，包括邻苯二甲酸酯、苯脲类除草剂和氨基甲酸酯类杀虫剂，研究了 TpAzo 的吸附机制。结果表明，TpAzo 与分析物之间的π堆积和疏水相互作用对吸附起重要作用。
