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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。
Objective To study the preparation and properties of sinomenine-β-cyclodextrin inclusion complex. Methods The inclusion complexes of sinomenine-β-cyclodextrin were prepared by solution blending method. The crystal forms of the inclusion complexes were observed by stereomicroscopy after purification. The crystal structures of the inclusion complexes were characterized by IR, DSC, X-ray powder diffraction (XRD) and nuclear magnetic resonance (1H-NMR) were used to characterize the inclusion complex. Results A new set of characteristic diffraction peaks was detected by XRD for sinomenine-β-CD inclusion complex with 2θ of 6.98 °, 8.48 °, 9.74 °, 9.92 ° and 18.50 °, respectively. There were obvious differences in the physical mixtures. Some characteristic absorption peaks of sinomenine were detected by IR, which were affected by the formation of inclusions, such as reduced intensity, widened peak shape, displacement or disappearance. The two protons, H-3 and H-5, on the inner wall of the lumen are affected by the inclusion formation and their chemical shifts are reduced. These characterization tests confirm that sinica-β-cyclodextrin inclusion has been formed. Conclusion Sinomenine and β-cyclodextrin can form a stable inclusion complex; β-cyclodextrin can significantly increase the solubility of sinomenine.