College of Chemistry and Molecular Sciences, Wuhan University, Wuhan, 430072, P. R. China.
Tobacco Research Institute of Hubei Province, Wuhan, 430040, P. R. China.
J Sep Sci. 2022 May;45(10):1746-1756. doi: 10.1002/jssc.202200055. Epub 2022 Mar 8.
An amino-functionalized magnetic covalent organic framework composite TpBD-(NH ) @Fe O (Tp=Tp1,3,5-triformylphloroglucinol, BD-(NH ) is 3,3',4,4'-biphenyltetramine) was prepared by post-synthesis modification. Due to its abundant benzene rings and amino groups, large specific surface area and porous structure, the prepared TpBD-(NH ) @Fe O exhibits high extraction efficiency toward sulfonylurea herbicides. Based on this, a new method of magnetic solid-phase extraction with TpBD-(NH ) @Fe O as the sorbent combined with high-performance liquid chromatography and ultraviolet detection was developed for trace analysis of sulfonylurea herbicides in environmental water, soil and tobacco leaves samples from tobacco land. Under the optimized conditions, the limits of detection within 0.05-0.14 μg/L were achieved with a high enrichment factor of 217-260-fold, and the relative standard deviations were 4.9-7.5% (n = 7, c = 0.5 μg/L). The linear range was around three orders of magnitude with the square of correlation coefficient higher than 0.9936. The method was applied to analyze five sulfonylurea herbicides in the environmental water, soil, and tobacco leave samples collected from tobacco land. No sulfonylurea herbicides were detected in these samples. The recoveries of target sulfonylurea herbicides in spiked environmental water, soil, and tobacco leaf samples were found in the range of 90.7-104, 70.7-99.0, and 59.3-97.8%, respectively. The results illustrate that the established TpBD-(NH ) @Fe O -magnetic solid-phase extraction- high-performance liquid chromatography-ultraviolet detection method is efficient for the analysis of trace sulfonylurea herbicides in environmental samples.
一种氨基功能化的磁性共价有机骨架复合材料 TpBD-(NH )@Fe O(Tp=Tp1,3,5-三(三氟甲基)苯并三嗪,BD-(NH )是 3,3',4,4'-联苯四胺)是通过后合成修饰制备的。由于其丰富的苯环和氨基、大的比表面积和多孔结构,所制备的 TpBD-(NH )@Fe O 对磺酰脲类除草剂表现出高的萃取效率。基于此,开发了一种以 TpBD-(NH )@Fe O 为吸附剂的新型磁性固相萃取方法,结合高效液相色谱和紫外检测,用于痕量分析环境水样、土壤和烟草叶样品中的磺酰脲类除草剂。在优化条件下,检测限在 0.05-0.14 μg/L 之间,富集因子为 217-260 倍,相对标准偏差为 4.9-7.5%(n=7,c=0.5 μg/L)。线性范围约为三个数量级,相关系数的平方大于 0.9936。该方法用于分析从烟草地采集的环境水样、土壤和烟草叶样品中的五种磺酰脲类除草剂。这些样品中均未检测到磺酰脲类除草剂。在环境水样、土壤和烟草叶样品中添加目标磺酰脲类除草剂的回收率分别为 90.7-104、70.7-99.0 和 59.3-97.8%。结果表明,建立的 TpBD-(NH )@Fe O-磁性固相萃取-高效液相色谱-紫外检测方法可有效分析环境样品中的痕量磺酰脲类除草剂。