College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China; College of Food Science and Technology, Hebei Agricultural University, Baoding 071001, China.
China Petroleum Engineering & Construction Corp. North China Company, Renqiu 062550, Hebei, China.
J Chromatogr A. 2023 Aug 2;1702:464087. doi: 10.1016/j.chroma.2023.464087. Epub 2023 May 19.
In this work, a series of 5,10,15,20-tetraphenylporphyrin (TPP)-based hyper crosslinked polymers were prepared by Friedel-Crafts reaction. Among them, the HCP-TPP-BCMBP, which was prepared by using TPP as the monomer and with 4,4'-Bis(chloromethyl)-1,1'-biphenyl (BCMBP) as the cross-linking agent, had the best adsorption capability for the enrichment of the nitroimidazoles of dimetridazole, ronidazole, secnidazole, metronidazole, and ornidazole. Then, a solid-phase extraction (SPE) method with the HCP-TPP-BCMBP as adsorbent coupled with HPLC-UV detection for the determination of nitroimidazole residues in honey, environmental water, and chicken breast samples was established. The influence of the main factors that affect the SPE, i.e., sample solution volume, sample loading rate, sample pH, and eluent and its volume, were studied. Under the optimal conditions, the limits of detection (S/N = 3) for the nitroimidazoles were measured to be in the range of 0.02-0.04 ng mL, 0.4-1.0 ng g and 0.5-0.7 ng g for environmental water, honey, and chicken breast samples, with the determination coefficients being in the range of 0.9933-0.9998. The analytes recoveries by the method in fortified samples fell in the range from 91.1% to 102.7% for environmental water, from 83.2% to 105.0% for honey, and from 85.9% to 103.0% for chicken breast samples, and the relative standard deviations for the determination were less than 10%. It shows that the HCP-TPP-BCMBP has a strong adsorption capability for some polar compounds.
在这项工作中,通过傅克反应制备了一系列 5,10,15,20-四苯基卟啉(TPP)基超交联聚合物。其中,以 TPP 为单体,以 4,4'-双(氯甲基)-1,1'-联苯(BCMBP)为交联剂制备的 HCP-TPP-BCMBP 对二甲硝唑、罗硝唑、塞克硝唑、甲硝唑和奥硝唑的硝基咪唑类化合物的富集具有最佳的吸附能力。然后,建立了以 HCP-TPP-BCMBP 为吸附剂的固相萃取(SPE)方法,结合高效液相色谱-紫外检测法,用于测定蜂蜜、环境水和鸡胸肉样品中的硝基咪唑残留量。研究了影响 SPE 的主要因素,如样品溶液体积、样品加载速率、样品 pH 值以及洗脱液及其体积。在最佳条件下,环境水、蜂蜜和鸡胸肉样品中硝基咪唑的检测限(S/N = 3)分别为 0.02-0.04ng mL、0.4-1.0ng g 和 0.5-0.7ng g,测定系数在 0.9933-0.9998 范围内。该方法在加标样品中的分析物回收率在环境水、蜂蜜和鸡胸肉样品中分别为 91.1%-102.7%、83.2%-105.0%和 85.9%-103.0%,测定的相对标准偏差均小于 10%。这表明 HCP-TPP-BCMBP 对一些极性化合物具有很强的吸附能力。