Sheikhzadeh M, Rohani S, Jutan A, Manifar T, Murthy K, Horne S
Department of Chemical and Biochemical Engineering, The University of Western Ontario, London, Ontario N6A 5B9, Canada.
Pharm Res. 2006 May;23(5):1043-50. doi: 10.1007/s11095-006-9779-6. Epub 2006 May 2.
The purpose of this study was to characterize Form 1 and Form 2 of buspirone hydrochloride, an anxiolytic medicine. The techniques used for characterization included microscopy (optical, hot stage, and scanning electron microscopy), thermal analysis (differential scanning calorimetry and thermogravimetric analysis), solid-state Fourier transform infrared (FTIR) spectroscopy, X-ray powder diffractometry (XRPD), and Raman spectroscopy. Morphologically, Form 1 and Form 2 consist of plate and columnar crystals, respectively, with good filterability. Thermal analysis showed that the two forms are enantiotropic over the studied temperature range. The FTIR method was used successfully for the quantification of Form 1 in a mixture of Forms 1 and 2. The ratio of a characteristic peak to a reference peak and the chemometric method were used to obtain the calibration curve. The Raman peak shifts showed the difference between the two forms especially for the n-butyl group. The large number of distinguishable XRPD peaks in the region of 5 degrees to 30 degrees 2theta of the two polymorphs demonstrated that XRPD is a useful tool for quantitative and qualitative analysis of polymorphs.
本研究的目的是对一种抗焦虑药物盐酸丁螺环酮的晶型1和晶型2进行表征。用于表征的技术包括显微镜检查（光学显微镜、热台显微镜和扫描电子显微镜）、热分析（差示扫描量热法和热重分析）、固态傅里叶变换红外（FTIR）光谱、X射线粉末衍射（XRPD）和拉曼光谱。从形态学上看，晶型1和晶型2分别由片状和柱状晶体组成，具有良好的过滤性。热分析表明，在研究的温度范围内，这两种晶型是互变异构的。FTIR方法成功用于定量分析晶型1和晶型2混合物中的晶型1。利用特征峰与参比峰的比值以及化学计量学方法获得校准曲线。拉曼峰位移显示了两种晶型之间的差异，特别是对于正丁基。两种多晶型物在5度至30度2θ范围内有大量可区分的XRPD峰，这表明XRPD是多晶型物定量和定性分析的有用工具。
