Guo Liying, Liu Jiajia, Li Jinqiu, Hao Lin, Liu Weihua, Wang Chun, Wu Qiuhua, Wang Zhi
College of Science, Hebei Agricultural University, Baoding 071001, China.
College of Science, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2021 Aug 16;1651:462301. doi: 10.1016/j.chroma.2021.462301. Epub 2021 May 28.
In this work, a core-shell structured magnetic covalent organic framework named as M-TpDAB was constructed with 3,3'-diaminobenzidine (DAB) and 1,3,5-triformylphloroglucinol (Tp) as building units. M-TpDAB was characterized by infrared spectroscopy, nitrogen adsorption-desorption isotherms, powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Using the M-TpDAB as adsorbent, a simple and highly effective method was proposed for preconcentrating phenylurea herbicides before high performance liquid-phase chromatography analysis. In the optimized conditions, a good linearity was achieved within the range of 0.15-100 ng mL for water sample, 1.0-100.0 ng mL for tea drink samples. The limits of detection for the analytes were 0.05-0.15 ng mL for water sample and 0.30-0.50 ng mL for drink samples. Satisfactory recoveries of spiked target compounds were in the range of 84.6%-105% for water sample and 80.3%-102% for tea drink samples. Finally, the M-TpDAB based method was successfully used to determine phenylurea herbicides in tea drinks and water samples, demonstrating a good alternative for analyzing trace level of phenylurea herbicides in water samples.
在本研究中,以3,3'-二氨基联苯胺(DAB)和1,3,5-三(对甲酰基苯基)间苯三酚(Tp)为构筑单元,构建了一种核壳结构的磁性共价有机框架,命名为M-TpDAB。通过红外光谱、氮气吸附-脱附等温线、粉末X射线衍射、扫描电子显微镜和透射电子显微镜对M-TpDAB进行了表征。以M-TpDAB作为吸附剂,提出了一种在高效液相色谱分析之前预富集苯基脲类除草剂的简单且高效的方法。在优化条件下,水样在0.15 - 100 ng/mL范围内、茶饮料样品在1.0 - 100.0 ng/mL范围内具有良好的线性关系。水样中分析物的检测限为0.05 - 0.15 ng/mL,饮料样品的检测限为0.30 - 0.50 ng/mL。加标目标化合物在水样中的回收率为84.6% - 105%,在茶饮料样品中的回收率为80.3% - 102%,令人满意。最后,基于M-TpDAB的方法成功用于测定茶饮料和水样中的苯基脲类除草剂,为分析水样中痕量苯基脲类除草剂提供了一种良好的替代方法。