Complex Formation between Deoxycholic Acid and Menabione by Grinding and Sealed Heating Methods

Complex Formation between Deoxycholic Acid and Menabione by Grinding and Sealed Heating Methods
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研磨和密封加热方法制备脱氧胆酸与甲烯那酮的络合物

DOI:
10.1248/cpb.45.1358
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发表时间:
1997
影响因子:
1.7
通讯作者:
Keiji. Yamamoto
Keiji. Yamamoto
中科院分区:
医学4区
文献类型:
--
作者:
S. Limmatvapirat;E. Yonemochi;T. Oguchi;Keiji. Yamamoto

文献摘要

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研究了去氧胆酸(DCA)与甲萘醌(MND)在研磨和密封加热条件下形成络合物的过程。通过共沉淀法制备了DCA与MND的配合物,其化学计量比为2:1(DCA:MND)。配合物的红外光谱表明,MND分子位于DCA分子形成的通道中。DCA-MND的10分钟研磨混合物给出与DCA-MND共沉淀物相同的X射线衍射图。差示扫描量热法(DSC)和红外光谱也证明了研磨混合物和络合物之间的相同结果,证实了DCA和MND之间通过研磨形成络合物。DSC数据表明,在DCA-MND物理混合物的加热过程中,预期会形成络合物。制备了密封加热样品,并与共沉淀法制备的配合物进行了比较。样品在110°C加热10 min或80°C加热24 h后,其X射线衍射图、DSC曲线和红外光谱与配合物相同。这些结果表明,在密封加热和研磨条件下,DCA和MND之间都发生了络合物的形成。
Complex formation between deoxycholic acid (DCA) and menadione (MND) by grinding and sealed heating was investigated. The complex between DCA and MND was prepared by coprecipitation and showed a stoichiometry of 2 : 1 (DCA : MND). The IR spectrum of the complex suggested that MND molecules were located in the channel formed by DCA molecules. The 10 min ground mixture of DCA-MND gave the same X-ray diffraction pattern as the DCA-MND coprecipitate. Differential scanning calorimetry (DSC) and IR spectroscopy also demonstrated the identical results between the ground mixture and the complex, confirming the complex formaiton between DCA and MND by grinding. The DSC data suggested that the complex formation was expected during heating process of the DCA-MND physical mixture. The sealed heated samples were prepared and compared with the complex prepared by coprecipitation. After heating in a sealed ampoule at 110°C for 10 min or at 80°C for 24h, samples demonstrated the same X-ray diffraction patterns, DSC curves and IR spectra as the complex. These results indicated that the complex formation took place between DCA and MND by sealed heating as well as by grinding.