College of Pharmacy, Key Laboratory of Public Health Safety of Hebei Province, Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, Hebei University, Baoding, 071002, China.
Anal Methods. 2022 Jan 27;14(4):401-409. doi: 10.1039/d1ay01954f.
Herein, a poly(ionic liquid@MOF) composite monolithic column was prepared radical polymerization using ionic liquid (1-allyl-3-methylimidazolium hexafluorophosphate) and MOF (derivatized UIO66-2COOH) as copolymer monomers. The composite monolithic column was characterized scanning electron microscopy (SEM), nitrogen adsorption-desorption isotherms and mercury intrusion porosimetry. Subsequently, the composite monolithic column combined with high performance liquid chromatography (HPLC) was used as a solid-phase extraction (SPE) absorbent for online purification and enrichment of tectochrysin in medicinal plants. The results indicated that the addition of the ionic liquid and MOF not only increased the surface area but also increased the adsorption capacity of the monolith for tectochrysin. The method showed good linearity in the concentration range of 0.01-500 μg mL. The calibration equation was = 2154.6 - 8.3785 and the limit of detection (LOD, S/N = 3) and the limit of quantification (LOQ, S/N = 10) were 3.33 ng mL and 10 ng mL, respectively. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.62%, the RSD of inter-column was less than 3.16%, and the recoveries ranged from 100.58% to 105.00%. Thus, results showed that this method is simple, accurate and convenient for the online enrichment and purification of tectochrysin from medicinal plants.
本文通过自由基聚合，以离子液体（1-烯丙基-3-甲基咪唑六氟磷酸盐）和 MOF（衍生化 UIO66-2COOH）为共聚单体，制备了一种聚（离子液体@MOF）复合整体柱。通过扫描电子显微镜（SEM）、氮气吸附-脱附等温线和压汞孔隙率对复合整体柱进行了表征。随后，将复合整体柱与高效液相色谱（HPLC）结合，作为固相萃取（SPE）吸附剂，用于在线净化和富集药用植物中的金钗石斛素。结果表明，离子液体和 MOF 的加入不仅增加了比表面积，而且提高了整体柱对金钗石斛素的吸附容量。该方法在 0.01-500 μg mL 的浓度范围内表现出良好的线性关系。校准方程为 y = 2154.6 - 8.3785，检测限（LOD，S/N = 3）和定量限（LOQ，S/N = 10）分别为 3.33 ng mL 和 10 ng mL。日内和日间精密度的相对标准偏差（RSD）小于 2.62%，柱间 RSD 小于 3.16%，回收率在 100.58%至 105.00%之间。因此，该方法简单、准确、方便，可用于药用植物中金钗石斛素的在线富集和净化。
