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 30;1679:463387. doi: 10.1016/j.chroma.2022.463387. Epub 2022 Jul 30.
Three magnetic covalent organic frameworks (named M-TpPa-SONa, M-TpPa-SOH and M-TpPa) were prepared by the solvothermal synthesis method with 1,3,5-trimethylphenol (TP) and either 2-sulfo-1,4-phenylenediamine (Pa-SOH) or p-phenylenediamine (Pa) as monomers. Among them, the M-TpPa-SONa possessed relatively high hydrophilicity, good magnetic responsiveness, and high affinity for the benzoylureas (BUs) insecticides. It was then explored as the magnetic solid-phase extraction adsorbent for the extraction of six BUs (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, flufenoxuron and chlorfluazuron) from water, pear juice and honey samples prior to high-performance liquid chromatography with ultraviolet detection. Under the optimized experimental conditions, a good linearity was achieved within the concentration range of 0.27-40.0 ng mL for water sample, 0.47-30.0 ng mL for pear juice sample, and 2.70-200.0 ng g for honey sample. The limits of detection for the analytes were 0.08-0.11 ng mL for water sample, 0.14-0.19 ng mL for pear juice sample and 0.80-1.00 ng g for honey sample. The method recoveries for spiked samples were in the range of 85.0%-111.0% with the relative standard deviations less than 8.8%. The developed method was successfully used for the determination of the BUs in water, pear juice and honey samples.
三种磁性共价有机框架(分别命名为 M-TpPa-SONa、M-TpPa-SOH 和 M-TpPa)采用溶剂热合成方法,以 1,3,5-三甲酚(TP)和 2-磺基-1,4-苯二胺(Pa-SOH)或对苯二胺(Pa)为单体制备。其中,M-TpPa-SONa 具有较高的亲水性、良好的磁响应性和对苯甲酰脲(BUs)杀虫剂的高亲和力。然后,它被探索作为磁性固相萃取吸附剂,用于从水样、梨汁和蜂蜜样品中萃取六种 BUs(除虫脲、伏虫隆、六氟隆、噻虫隆、氟虫脲和氯氟脲),然后进行高效液相色谱法结合紫外检测。在优化的实验条件下,水样的浓度范围为 0.27-40.0ng mL 时呈现良好的线性,梨汁样品的浓度范围为 0.47-30.0ng mL,蜂蜜样品的浓度范围为 2.70-200.0ng g。各分析物的检出限为水样 0.08-0.11ng mL,梨汁样品 0.14-0.19ng mL,蜂蜜样品 0.80-1.00ng g。加标样品的方法回收率在 85.0%-111.0%范围内,相对标准偏差小于 8.8%。该方法成功用于水样、梨汁和蜂蜜样品中 BUs 的测定。