Reevaluation of solubility of tolbutamide and polymorphic transformation from Form I to unknown crystal form.
Reevaluation of solubility of tolbutamide and polymorphic transformation from Form I to unknown crystal form.
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DOI：
10.1016/j.ijpharm.2008.10.018
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发表时间：
2009-03
影响因子：
5.8
通讯作者：
Gen Hasegawa;Takao Komasaka;R. Bando;Y. Yoshihashi;E. Yonemochi;K. Fujii;H. Uekusa;K. Terada
中科院分区：
文献类型：
--
作者：
Gen Hasegawa;Takao Komasaka;R. Bando;Y. Yoshihashi;E. Yonemochi;K. Fujii;H. Uekusa;K. Terada
使用量热法和光谱分析评估多晶型物之间的甲苯磺丁脲的热力学稳定性顺序。 I-III 型的溶解热 (ΔH) 测量是在二甲基亚砜中于 298.2K 至 319.2K 之间进行的。发现形式II和III的ΔH几乎与温度升高平行地增加。然而，晶型I的ΔH随温度升高的变化与其他晶型的变化并不对应。溶解度数据证实了 I 型的 ΔH 变化在 308.2K 左右。晶型 I 的 XRD-DSC 测量检测到在 311K 时发生多晶型转变（晶型 IL→未知晶型）。获得的数据表明，在311K以上将存在新晶型(Form IH)，并且在转变温度以下，热力学稳定性顺序为“Form III<Form IL<Form II”，而在转变温度以上，则顺序变为“Form IL和Form IH<Form III<Form II”。通过在SPring-8上测量BL19B2上的PXRD图谱确定了IH型的晶体结构，并且固态NMR谱的变化证实了IL型晶体结构的转变。
Thermodynamic stability order of tolbutamide between polymorphs was evaluated using calorimetry and spectroscopic analysis. The heat of solution (ΔH) of Forms I–III measurements were carried out in dimethylsulfoxide between 298.2K and 319.2K. It was found that the ΔH of Forms II and III was increased nearly parallel with a temperature rise. However, change of the ΔH of Form I with a temperature rise was not in correspondence with that of other forms. Solubility data confirmed the change in ΔH of Form I around 308.2K. XRD–DSC measurement of Form I detected a polymorphic transformation (Form IL→unknown form) at 311K. Obtained data suggested that the new crystal form (Form IH) would exist above 311K, and the order of thermodynamic stability was “Form III<Form IL<Form II” below the transition temperature, on the other hand, the order was changed in “Form ILand Form IH<Form III<Form II” above the transition temperature. The crystal structure of Form IHwas determined by measurement of PXRD pattern on BL19B2 at SPring-8, and the change in the solid-state NMR spectrum confirmed the transformation of the crystal structure of Form IL.