Department of Chemistry, College of Science, Hebei Agricultural University, Baoding 071001, China.
Department of Chemistry, College of Science, Hebei Agricultural University, Baoding 071001, China; Department of Food Science, College of Food Science and Technology, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2022 Aug 2;1676:463206. doi: 10.1016/j.chroma.2022.463206. Epub 2022 Jun 9.
The three hypercrosslinked polymers (HCP) materials, designated as OPD-HCP, MPD-HCP and PPD-HCP, were synthesized by using o-phenylenediamine (OPD), m-phenylenediamine (MPD) and p-phenylenediamine (PPD) as monomers. They were characterized by infrared spectroscopy, powder X-ray diffraction, nitrogen sorption isotherms, and scanning electron microscopy. Then, the HCPs were explored as solid-phase extraction (SPE) adsorbent for the extraction of five nitroimidazoles (NDZs) (metronidazole, ronidazole, secnidazole, dimetridazole and ornidazole). Among the three HCPs, the MPD-HCP has the best adsorption performance for the NDZs. With the help of high-performance liquid chromatography with ultraviolet detection (HPLC-UV), good linear response range (0.07-40.0 ng mL), high method recovery (86.8%-113.3%), low limits of detection (0.02-0.15 ng mL) and good precision with the relative standard deviations of less than 8.1% were achieved for the determination of the NDZs in water samples. The effective determination of the NDZs in peach juice, honey tea, and honey samples were also realized by the developed method with satisfactory results. Based on both the experimental results and density functional theory calculation, the adsorption mechanism can be attributed to multiple interactions between the MPD-HCP and the NDZs, including hydrogen bonding, hydrophilic, and electrostatic interactions. The method provides a new alternative of choice for the determination of some NDZs in real samples.
三种超交联聚合物（HCP）材料，分别命名为 OPD-HCP、MPD-HCP 和 PPD-HCP，以邻苯二胺（OPD）、间苯二胺（MPD）和对苯二胺（PPD）为单体合成。通过红外光谱、粉末 X 射线衍射、氮气吸附等温线和扫描电子显微镜对其进行了表征。然后，将 HCP 作为固相萃取（SPE）吸附剂，用于萃取五种硝基咪唑类（NDZs）（甲硝唑、罗硝唑、塞克硝唑、二甲硝唑和奥硝唑）。在这三种 HCP 中，MPD-HCP 对 NDZs 的吸附性能最好。在高效液相色谱-紫外检测（HPLC-UV）的帮助下，该方法实现了良好的线性响应范围（0.07-40.0ng/mL）、高方法回收率（86.8%-113.3%）、低检测限（0.02-0.15ng/mL）和小于 8.1%的相对标准偏差的精度，可用于水样中 NDZs 的测定。通过开发的方法还可以有效测定桃汁、蜂蜜茶和蜂蜜样品中的 NDZs，结果令人满意。基于实验结果和密度泛函理论计算，吸附机制可归因于 MPD-HCP 和 NDZs 之间的多种相互作用，包括氢键、亲水性和静电相互作用。该方法为实际样品中某些 NDZs 的测定提供了一种新的选择。
