Lv Yongqin, Hughes Timothy C, Hao Xiaojuan, Mei Danping, Tan Tianwei
Beijing Key Laboratory of Bioprocess, College of Life Science and Technology, Beijing University of Chemical Technology, Beijing, P. R. China; Materials Science and Engineering, CSIRO, Melbourne, VIC, Australia.
J Sep Sci. 2011 Aug;34(16-17):2131-7. doi: 10.1002/jssc.201100282. Epub 2011 Jul 18.
Monomeric and epichlorohydrin polymerized β-CD functionalized monoliths were prepared for the rapid isolation and purification of the isoflavonoid puerarin, a well-known traditional Chinese drug, from a crude extract of Radix puerariae (root of the plant Pueraria lobata). Two copolymers poly(isocyanatoethyl methacrylate-co-methyl methacrylate-co-ethylene dimethacrylate) (poly(IEM-co-MMA-co-EDMA)) and poly(glycidyl methacrylate-co-EDMA) (poly(GMA-co-EDMA)) were developed as facile, highly reactive and versatile monolithic matrix. SEM characterization demonstrated that the modified monoliths had homogenous porous structure and morphology. The success of the chemical modification of the monolithic matrix was confirmed by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), solid-state (13) C NMR and elemental analysis. It was demonstrated that polymeric β-CD modified monoliths had better separation and selectivity for puerarin, recovering puerarin with a purity of 96% (m%) and a yield of 93% (m%). Compared with poly(glycidyl methacrylate-co-EDMA), poly(isocyanatoethyl methacrylate-co-methyl methacrylate-co-EDMA) monolithic matrix had higher reactivity, which significantly improved the β-CD ligand density and thus the selectivity of the monoliths. Puerarin with a purity of 96% (m%) and with a yield of 89% (m%) was recovered on the monolith.
制备了单体和环氧氯丙烷聚合的β-环糊精功能化整体柱,用于从葛根(植物野葛的根)粗提物中快速分离和纯化著名的传统中药异黄酮葛根素。开发了两种共聚物聚(甲基丙烯酸异氰酸乙酯-共-甲基丙烯酸甲酯-共-二甲基丙烯酸乙烯酯)(聚(IEM-共-MMA-共-EDMA))和聚(甲基丙烯酸缩水甘油酯-共-EDMA)(聚(GMA-共-EDMA))作为简便、高反应性和通用的整体柱基质。扫描电子显微镜表征表明,改性后的整体柱具有均匀的多孔结构和形态。通过傅里叶变换红外光谱(FTIR)、差示扫描量热法(DSC)、固态(13)C核磁共振和元素分析证实了整体柱基质化学改性的成功。结果表明,聚合物β-环糊精改性整体柱对葛根素具有更好的分离性能和选择性,回收的葛根素纯度为96%(质量分数),收率为93%(质量分数)。与聚(甲基丙烯酸缩水甘油酯-共-EDMA)相比,聚(甲基丙烯酸异氰酸乙酯-共-甲基丙烯酸甲酯-共-EDMA)整体柱基质具有更高的反应活性,显著提高了β-环糊精配体密度,从而提高了整体柱的选择性。在该整体柱上回收的葛根素纯度为96%(质量分数),收率为89%(质量分数)。