使用傅里叶变换拉曼光谱法对结晶度进行定量分析。
The quantitative analysis of crystallinity using FT-Raman spectroscopy.
作者信息
Taylor L S, Zografi G
机构信息
School of Pharmacy, University of Wisconsin-Madison, 53706, USA.
出版信息
Pharm Res. 1998 May;15(5):755-61. doi: 10.1023/a:1011979221685.
PURPOSE
To establish if FT-Raman spectroscopy can be used to quantitate the degree of crystallinity in a model compound.
METHODS
Mixtures containing different proportions of amorphous and crystalline indomethacin were prepared. Using the peak intensity ratio 1698 cm(-1) (crystalline) to 1680 cm(-1) (amorphous), a correlation curve was prepared. This correlation curve was validated by testing further samples of known composition. Partially crystalline indomethacin was prepared by milling crystalline indomethacin.
RESULTS
A linear correlation curve was obtained across the entire range of 0-100% crystallinity. Using this method, it was possible to detect down to either 1% amorphous or crystalline content. The largest errors were found to result from inhomogeneities in the mixing of the calibration and validation samples. The spectra of the mechanically processed samples were similar to the spectra of the calibration samples, and the degree of crystallinity could be estimated in these samples.
CONCLUSIONS
FT-Raman spectroscopy is a potentially useful method to complement existing techniques for the quantitative determination of crystallinity.
目的
确定傅里叶变换拉曼光谱法是否可用于定量分析模型化合物的结晶度。
方法
制备含有不同比例无定形和结晶型吲哚美辛的混合物。利用1698 cm⁻¹（结晶型）与1680 cm⁻¹（无定形）的峰强度比绘制相关曲线。通过测试已知组成的其他样品对该相关曲线进行验证。通过研磨结晶型吲哚美辛制备部分结晶型吲哚美辛。
结果
在0 - 100%结晶度的整个范围内获得了线性相关曲线。使用该方法，能够检测低至1%的无定形或结晶含量。发现最大误差源于校准和验证样品混合不均匀。机械加工样品的光谱与校准样品的光谱相似，并且可以估计这些样品的结晶度。
结论
傅里叶变换拉曼光谱法是一种潜在有用的方法，可补充现有用于定量测定结晶度的技术。
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