Microchimica Acta ( IF 5.3 ) Pub Date : 2021-06-09 , DOI: 10.1007/s00604-021-04852-8 Yanyan Xing 1 , Jianshu Li 2 , Meiling Chen 1 , Xiangting Wang 1 , Xiaohong Hou 2
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A novel magnetic borate-functionalized metal-organic framework nanocomposite was designed and fabricated for selective enrichment of catecholamines from human urine. Firstly, the polytannic acid (PTA) layer with natural low-cost and ecofriendly polyphenol tannic acid as the organic ligand and Fe3+ as the cross-linker was coated onto the surface of Fe3O4. Then, the borate-functionalized metal-organic framework (MIL-100(Fe)-B) with 5-boronobenzene-1,3-dicarboxylic acid as a ligand fragment was modified onto the PTA-coated Fe3O4 through a metal-ligand-fragment coassembly strategy. The obtained smart porous adsorbent Fe3O4@PTA@MIL-100(Fe)-B was confirmed by means of several characterization methods and then applied as an effective magnetic solid phase extraction (MSPE) sorbent for specific extraction of trace catecholamines in human urine. The Plackett–Burman design was used for screening the variables significantly affecting the extraction efficiency. Then, the significant factors were further investigated by the Box–Behnken design to determine the optimal extraction conditions. Under the optimal conditions, a method for selective MSPE combined with high-performance liquid chromatography with a fluorescence detector for the quantitation of catecholamines in human urine was developed and validated. With the proposed method, the linearity range was from 0.500 to 500 ng mL−1 for norepinephrine and epinephrine and from 1.00 to 500 ng mL−1 for dopamine. The detection limits were 0.050, 0.11, and 0.20 ng mL−1 for norepinephrine, epinephrine, and dopamine, respectively. The recoveries from spiking experiments varied from 91.5 to 108% with relative standard deviations (RSDs) of 0.80–4.8%. The established method is rapid, sensitive, accurate, inexpensive, and ecofriendly and was successfully applied to the determination of the target catecholamines in human urine samples.
Graphical abstract
中文翻译：
单宁酸定向合成磁性和硼酸功能化金属有机骨架，用于选择性提取和定量人尿中的儿茶酚胺
设计并制造了一种新型磁性硼酸盐功能化金属有机骨架纳米复合材料，用于选择性富集人尿中的儿茶酚胺。首先，以天然低成本、环保的多酚单宁酸为有机配体，Fe 3+为交联剂，将聚单宁酸(PTA)层包覆在Fe 3 O 4表面。然后，硼酸官能金属-有机骨架（MIL-100（铁）-B）与5- boronobenzene -1,3-二羧酸作为配体片段被修改到PTA-包Fe 3 ö 4通过金属配体-片段共组装策略。得到的智能多孔吸附剂Fe 3 O 4@PTA@MIL-100(Fe)-B 通过多种表征方法得到证实，然后用作有效的磁性固相萃取 (MSPE) 吸附剂，用于特定提取人尿中的痕量儿茶酚胺。Plackett-Burman 设计用于筛选显着影响提取效率的变量。然后，通过 Box-Behnken 设计进一步研究重要因素以确定最佳提取条件。在最佳条件下，开发并验证了选择性 MSPE 结合带有荧光检测器的高效液相色谱定量人尿中儿茶酚胺的方法。使用建议的方法，线性范围为 0.500 至 500 ng mL -1对于去甲肾上腺素和肾上腺素，多巴胺从 1.00 到 500 ng mL -1。去甲肾上腺素、肾上腺素和多巴胺的检测限分别为 0.050、0.11 和 0.20 ng mL -1。加标实验的回收率从 91.5% 到 108% 不等，相对标准偏差 (RSD) 为 0.80–4.8%。所建立的方法具有快速、灵敏、准确、廉价、环保等特点，已成功应用于人尿样中目标儿茶酚胺的测定。
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