Key Laboratory of Pharmaceutical Quality Control of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China; Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Baoding 071002, China.
Key Laboratory of Pharmaceutical Quality Control of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China; Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Baoding 071002, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Sep 1;1125:121715. doi: 10.1016/j.jchromb.2019.121715. Epub 2019 Jul 9.
A metal organic framework (MOF)-polymer monolithic column was prepared by redox initiation using modified MOF and N-methylolacrylamide (NMA) as co-monomers. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption isotherm measurement. It was used as a solid phase extraction (SPE) absorbent for the online enrichment of ursolic acid (UA) by high performance liquid chromatography. The adsorption amount of UA on the monolith was compared with that of silica gel-C18 adsorbent and the monolith without MOF material. The MOF-polymer monolithic column showed high selectivity and good permeability. Under the optimum conditions for extraction and determination, the calibration equation was y = 79.854× + 0.1939; the linear range was 0.001-0.9 mg/mL; the linear regression coefficient was 0.9993; the limit of detection (LOD) and the limit of quantification (LOQ) were 0.17 μg/mL and 0.57 μg/mL, respectively; the inter-day and intra-day accuracies were <6.44%; the recovery was in the range of 86.52-105.26%. The MOF-polymer monolithic column was successfully used as SPE column for enrichment and determination of UA in Chinese herbal medicine.
采用氧化还原引发剂，以改性金属有机骨架（MOF）和 N-羟甲基丙烯酰胺（NMA）为共聚单体制备 MOF-聚合物整体柱。通过扫描电子显微镜（SEM）和氮气吸附-脱附等温线测量对所得整体柱进行了表征。将其用作高效液相色谱法在线富集熊果酸（UA）的固相萃取（SPE）吸附剂。比较了 UA 在整体柱上的吸附量与硅胶-C18 吸附剂和无 MOF 材料的整体柱上的吸附量。MOF-聚合物整体柱表现出高选择性和良好的渗透性。在萃取和测定的最佳条件下，校准方程为 y = 79.854× + 0.1939；线性范围为 0.001-0.9 mg/mL；线性回归系数为 0.9993；检测限（LOD）和定量限（LOQ）分别为 0.17 μg/mL 和 0.57 μg/mL；日内和日间精密度均<6.44%；回收率在 86.52-105.26%范围内。MOF-聚合物整体柱成功用作 SPE 柱，用于富集和测定中草药中的 UA。
