Department of Chemistry, College of Science, Hebei Agricultural University, Baoding, Hebei 071001, China.
College of Food Science and Technology, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2022 Jun 21;1673:463077. doi: 10.1016/j.chroma.2022.463077. Epub 2022 Apr 25.
In this work, a porous extended network covalent organic framework designated as TP-NDA-COF was synthesized by the reaction of 2,4,6-trihydroxy-benzene-1,3,5-tricarbaldehyde (TP) and 1,5-naphthalenediamine (NDA). The structure and morphology of the TP-NDA-COF was characterized by means of Fourier transform infrared spectra (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscope (SEM). The TP-NDA-COF was applied as a solid-phase extraction adsorbent for the extraction of some chlorophenols from water and lemon black tea beverage samples prior to high performance liquid chromatography-UV detection. The main experimental parameters that affect the extraction efficiency including the type and volume of eluent, sample solution volume, sample loading rate and sample solution pH were investigated. Under the optimal conditions, the calibration curves were linear in the range of 0.30-60.0 ng mL with the determination coefficients (R) of 0.9996-0.9998 for water samples and in the range of 0.60-60.0 ng mL with the R values from 0.9990 to 0.9996 for beverage samples. At the signal to noise ratio of 3 (S/N = 3), the method LODs for the analytes were 0.10-0.15 ng mL for water samples and 0.20-0.50 ng mL for lemon black tea beverage, respectively. Good repeatability was achieved with the relative standard deviations of less than 7%. The results showed that the SPE-HPLC method can be used for the determination of chlorophenols in environmental water and foodstuffs samples.
在这项工作中，通过 2,4,6-三羟基-苯-1,3,5-三甲醛（TP）和 1,5-萘二胺（NDA）的反应，合成了一种多孔扩展网络共价有机骨架，命名为 TP-NDA-COF。通过傅里叶变换红外光谱（FT-IR）、热重分析（TGA）、X 射线衍射（XRD）和扫描电子显微镜（SEM）对 TP-NDA-COF 的结构和形态进行了表征。将 TP-NDA-COF 用作固相萃取吸附剂，用于从水样和柠檬黑茶饮料样品中萃取一些氯酚，然后进行高效液相色谱-紫外检测。研究了影响萃取效率的主要实验参数，包括洗脱剂的类型和体积、样品溶液体积、样品加载速率和样品溶液 pH 值。在最佳条件下，校准曲线在水样中为 0.30-60.0ng mL 范围内呈线性，相关系数（R）为 0.9996-0.9998；在饮料样品中为 0.60-60.0ng mL 范围内呈线性，相关系数（R）为 0.9990-0.9996。在信噪比为 3（S/N=3）时，分析物的方法检出限（LOD）为 0.10-0.15ng mL，用于水样；0.20-0.50ng mL，用于柠檬黑茶饮料。相对标准偏差小于 7%，重复性良好。结果表明，SPE-HPLC 法可用于测定环境水样和食品中氯酚的含量。
