Low- versus Mid-frequency Raman Spectroscopy for in Situ Analysis of Crystallization in Slurries

拉曼光谱 原位 结晶 泥浆 光谱学 材料科学 分析化学(期刊) 化学 化学工程 结晶学 物理 色谱法 光学 工程类 有机化学 复合材料 量子力学
作者
Jaana Koskela,Joshua J. Sutton,Tiina Lipiäinen,Keith C. Gordon,Clare J. Strachan,Sara J. Fraser‐Miller
出处
期刊:Molecular Pharmaceutics [American Chemical Society]
卷期号:19 (7): 2316-2326 被引量:3
标识
DOI:10.1021/acs.molpharmaceut.2c00126
摘要

Slurry studies are useful for exhaustive polymorph and solid-state stability screening of drug compounds. Raman spectroscopy is convenient for monitoring crystallization in such slurries, as the measurements can be performed in situ even in aqueous environments. While the mid-frequency region (400-4000 cm-1) is dominated by intramolecular vibrations and has traditionally been used for such studies, the low-frequency spectral region (<200 cm-1) probes solid-state related lattice vibrations and is potentially more valuable for understanding subtle and/or complex crystallization behavior. The aim of the study was to investigate low-frequency Raman spectroscopy for in situ monitoring of crystallization of an amorphous pharmaceutical in slurries for the first time and directly compare the results with those simultaneously obtained with mid-frequency Raman spectroscopy. Amorphous indomethacin (IND) slurries were prepared at pH 1.2 and continuously monitored in situ at 5 and 25 °C with both low- and mid-frequency Raman spectroscopy. At 25 °C, both spectral regions profiled amorphous IND in slurries as converting directly from the amorphous form toward the α crystalline form. In contrast, at 5 °C, principal component analysis revealed a divergence in the detected conversion profiles: the mid-frequency Raman suggested a direct conversion to the α crystalline form, but the low-frequency region showed additional transition points. These were attributed to the appearance of minor amounts of the ε-form. The additional solid-state sensitivity of the low-frequency region was attributed to the better signal-to-noise ratio and more consistent spectra in this region. Finally, the low-frequency Raman spectrum of the ε-form of IND is reported for the first time.
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