结晶
差示扫描量热法
结晶度
热重分析
无定形固体
化学工程
傅里叶变换红外光谱
材料科学
结晶水
热稳定性
化学
结晶学
有机化学
热力学
物理
工程类
作者
Rong Qi,Hongxun Hao,Na Wang,Ting Wang,Lina Zhou,Guoliang Zhu,Haoran Mei,Ailing Liu,Yaling Li,Xin Huang
标识
DOI:10.1021/acs.cgd.3c01436
摘要
Amorphous tilmicosin phosphate (TMP) suffers from low stability, and its crystalline product is not reported. At the same time, the gelation phenomenon often occurs in the crystallization process of TMP, which seriously affects the robustness of the process and product quality. In this paper, a crystal form of TMP was developed, and it was determined to be tilmicosin phosphate trihydrate by powder X-ray diffraction, thermogravimetric differential scanning calorimetry, Fourier transform infrared (FTIR), and Karl Fischer water content test. Besides, the gelation phenomenon and the gel transition process during TMP crystallization were studied by spectroscopic and microscopic methods. The results show that TMP gel is an intermediate form formed by amorphous TMP and solvent, and the type of solvents and water content in these solvents were important factors affecting the gelation and crystallization behavior of TMP. Finally, the TMP crystallization process was optimized, and trihydrate of TMP could be obtained directly without passing through the intermediate gel state. It was found that, after process optimization, the particle size, crystallinity, and stability of the obtained crystal products were improved.
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