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首页> 外文期刊>Crystal growth & design >An Investigation into the Dehydration Behavior of Paroxetine HCl Form I Using a Combination of Thermal and Diffraction Methods: The Identification and Characterization of a New Anhydrous Form
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An Investigation into the Dehydration Behavior of Paroxetine HCl Form I Using a Combination of Thermal and Diffraction Methods: The Identification and Characterization of a New Anhydrous Form

机译：结合热和衍射方法研究帕罗西汀盐酸盐I的脱水行为：一种新型无水形式的鉴定和表征

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摘要

Paroxetine HCl can exist as a nonstoichiometric hydrate (Form II) or as a stoichiometric hemihydrate (Form I); the latter is considered to be the stable form and its structure is well-known. However, little work has been performed to investigate its dehydration behavior; hence, the generation of the anhydrous form via dehydration of Form I was investigated. A combination of thermal (differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA)) and diffraction (variabletemperature X-ray powder diffraction (VT-XRPD)) techniques was used. Dehydrated Form I was prepared using ultradry conditions, and the resulting product was compared to dehydrated Form II. DSC indicated that the two dehydrated forms of Forms I and II had distinct melting points. TGA experiments allowed the calculation of the activation energy for the dehydration of Form I, which varies between 86 and 114 kJ/mol. Pawley refinement of the VT-XRPD data suggested that Form I dehydrates to an isostructural anhydrate, since the unit cell parameters of this new form were very similar to those of Form I with only a smaller volume as a consequence of dehydration. Comparison with dehydrated Form II indicated that these two forms represent different crystal entities; hence, a new anhydrous form of paroxetine HCl has been identified.
机译：盐酸帕罗西汀可以非化学计量的水合物（形式II）或化学计量的半水合物（形式I）存在;后者被认为是稳定形式，其结构是众所周知的。但是，几乎没有工作来研究其脱水行为。因此，研究了通过形式I的脱水产生无水形式。使用了热技术（差示扫描量热法（DSC）和热重分析（TGA））和衍射技术（可变温度X射线粉末衍射（VT-XRPD））技术。使用超干条件制备脱水形式I，并将所得产物与脱水形式II进行比较。 DSC表明形式I和II的两种脱水形式具有不同的熔点。 TGA实验允许计算形式I脱水的活化能，该活化能在86至114 kJ / mol之间变化。 VT-XRPD数据的Pawley改进表明，形式I脱水为同构无水物，因为这种新形式的晶胞参数与形式I的晶胞参数非常相似，仅因脱水而体积较小。与脱水形式II的比较表明，这两种形式代表不同的晶体实体。因此，已经确定了一种新的无水形式的盐酸帕罗西汀。

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