Acta Pharm. 2014 Mar;64(1):1-13. doi: 10.2478/acph-2014-0009.
Crystallization of the drug entacapone from binary solvent mixtures was monitored in situ using a Raman optical probe. The recorded Raman spectra and statistical analysis, which included the principal components method and indirect hard modeling made it possible to estimate the starting point of crystallization, to assess crystallization temperatures and to provide information on the polymorphic content of the mixture. It was established that crystallization temperatures were proportional to the volume content of the solvent in mixtures. The samples were also evaluated off-line via Raman spectroscopy and SWAXS. The collected data showed the presence of forms b and g in all solvent mixtures. In a toluene/methanol 30:70 mixture, in addition to forms b and g, at least one of the forms A, D or a was also indicated by SWAXS. The results have shown that the presence of a particular polymorph is strongly dependent on the nature and portion of the solvent in the binary solvent mixture.
采用拉曼光学探头原位监测二元溶剂混合物中药物恩他卡朋的结晶过程。记录的拉曼光谱和统计分析（包括主成分法和间接硬建模）可用于估算结晶起始点、评估结晶温度，并提供混合物中多晶型物含量的信息。结果表明，结晶温度与混合物中溶剂的体积含量成正比。还通过拉曼光谱和 SWAXS 对样品进行了离线评估。收集的数据表明，所有溶剂混合物中均存在形式 b 和 g。在甲苯/甲醇 30:70 的混合物中，除形式 b 和 g 外，SWAXS 还表明至少存在形式 A、D 或 a 中的一种。结果表明，特定多晶型物的存在强烈取决于二元溶剂混合物中溶剂的性质和比例。
