[关键词]
[摘要]
目的 研究青藤碱-β-环糊精包合物的制备与性质。方法 通过溶液共混法制备青藤碱-β-环糊精包合物,纯化后利用体式显微镜观察各包合物的结晶形态,并通过红外光谱(IR)、差热分析(DSC)、X射线粉末衍射(XRD)、核磁共振氢谱(1H-NMR)等方法对包合物进行表征。结果 对青藤碱-β-CD包合物,XRD检测到一组新的特征衍射峰,2θ分别为6.98°、8.48°、9.74°、9.92°、18.50°;DSC能观察到包合物与物理混合物存在明显不同;IR检测到青藤碱的部分特征吸收峰,受包合物形成的影响其强度降低,峰形变宽,发生位移或消失等现象;1H-NMR能检测到β-CD空腔内壁的两个质子H-3和H-5受包合物形成的影响其化学位移减小。这些表征试验均证实,青藤碱-β-环糊精包合物已经形成。结论 青藤碱与β-环糊精可形成稳定的包合物;β-环糊精可显著增加青藤碱的溶解度。
[Key word]
[Abstract]
Objective To investigate the preparation and characterizations of the inclusion complex of sinomenine (SN) with β-cyclodextrin (β-CD). Methods The inclusion complex of SN-β-CD was successfully prepared by mixed solution method, then the crystalline morphology and micromorphology of the inclusion complex were characterized and analyzed by stereomicroscope after purification and recrystallization. X-ray diffraction (XRD), infrared spectrography (IR), differential scanning caborimetry (DSC), and hydrogen nuclear magnetic resonance (1H-NMR) were used to characterize the structure and the properties of the inclusion complex. Results A group of new features diffraction peaks at 6.98°, 8.48°, 9.74°, 9.92°, and 18.50° of the inclusion complex were detected by XRD; The DSC data suggested that there was obvious difference between inclusion complex and the physical mixed samples of SN- β-CD; IR spectra showed that the intensity of a few characteristic absorption peaks of SN decreased, and the peak shape was widened and the displacement was changed or disappeared by the influence of inclusion complex; 1H-NMR spectra indicated that the chemical shift of H-3 and H-5 in the intine of β-CD could be determined due to the formation of the inclusion complex. All these characteristics confirmed that the inclusion complex of SN-β-CD was formed. Conclusion SN and β-CD could form stable inclusion complex, and β-CD could sharply increase the solubility of SN.
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[基金项目]
湖南省自然科学基金资助项目(06JJ50020);民族药用植物资源研究与利用湖南省重点实验室开放基金项目(HHUW2010-68)