柚皮素与卡马西平共晶的红外光谱与拉曼光谱分析

Infrared and Raman Spectrum of Naringin-Carbamazepine Cocrystal

目的采用红外光谱和拉曼光谱探讨柚皮素与卡马西平共晶的形成机制和弱相互作用的关系。方法通过悬浮液法制备柚皮素与卡马西平共晶样品,采用X射线衍射法(XRD)对共晶样品进行表征,确证所得样品为共晶物纯品。采用傅里叶变换红外光谱法(FTIR)和拉曼光谱法(Raman)对共晶样品进行分析,并与药物活性成分(API)、共晶形成物(CCF)的红外光谱及拉曼光谱进行比对分析。结果柚皮素与卡马西平共晶的红外特征吸收峰和拉曼位移均产生了峰位置偏移以及峰强度的变化,主要体现在红外波数的3500~3000 cm^(-1)范围内与杂原子相连接氢原子的伸缩振动变化明显,如-NH_(2)和-OH的特征峰向低频移动且峰有变宽的趋势;拉曼位移在1000~800 cm^(-1)波数范围内苯环的基频振动峰发生变化。结论红外光谱与拉曼光谱在共晶物质鉴别分析与分子作用力分析研究中具有良好应用,光谱分析获得的分子间作用力信息,如红外光谱的-OH伸缩振动峰和-C-N伸缩振动峰偏移,拉曼光谱得出二者分子之间存在氢键、π-π堆积等相互作用力,与共晶的形成机制一致,并与其单晶结构的分析相吻合,印证了基于光谱探测共晶成因的研究具有较好可行性,可为阐明共晶形成机制与特点提供较全面的、多维度的科学依据。

Objective To probe into the formation mechanism and weak interaction between naringin and carbamazepine cocrystal was studied by infrared and Raman spectroscopy.Methods Fixed stoichiometry cocrystals of naringin with carbamazepine were prepared by solvent-assisted grinding.The cocrystal samples were quickly and effectively characterized by powder X-ray diffraction(PXRD),infrared and Raman spectum.The potential mechanism of cocrystal formation was discussed by analyzing the changes of intermolecular interaction.Results The infrared characteristic absorption peak and Raman shift of naringin and carbamazepine cocrystal produce the shift of peak position and the change of peak height and peak width,which is mainly reflected in the obvious change of stretching vibration of hydrogen atom in the range of 3500-3000 cm^(-1) of infrared wave number.For example,the characteristic peaks of-NH_(2) and-OH move to low frequency number and tend to widen.The fundamental frequency vibration peak of benzene ring changes in the wavelength range of 1000-800 cm^(-1) of Raman wave number.Conclusion Infrared spectrum and Raman spectrum can be used for the identification and analysis of cocrystal materials.The intermolecular force information obtained by spectral analysis,such as the shift of-OH stretching vibration peak and-C-N stretching vibration peak in infrared spectrum,and the interaction forces such as hydrogen bond andπ-πaccumulation between the two molecules in Raman spectrum,which is consistent with the formation mechanism of cocrystal and the analysis of single crystal structure,which proves that the research on the origin of cocrystal based on spectrum is feasible,and provides a comprehensive and multi-dimensional scientific basis for clarifying the formation mechanism and characteristics of cocrystal.