Dry and Wet Mechanochemical Synthesis of Piroxicam and Saccharin Co-Crystals and Evaluation by Powder X-Ray Diffraction, Thermal Analysis and Mid- and Near- Infrared Spectroscopy
Dry and Wet Mechanochemical Synthesis of Piroxicam and Saccharin Co-Crystals and Evaluation by Powder X-Ray Diffraction, Thermal Analysis and Mid- and Near- Infrared Spectroscopy
复制标题
吡罗昔康和糖精共晶的干法和湿法机械化学合成以及粉末 X 射线衍射、热分析和中近红外光谱评价
DOI：
10.1016/j.xphs.2021.06.024
复制
发表时间：
2022
影响因子：
3.8
通讯作者：
Goto Satoru
中科院分区：
文献类型：
--
作者：
Otsuka Yuta;Goto Satoru
本研究的目的是考察干法和湿法机械力化学合成对吡罗昔康(PX)和糖精(SA)混合物的影响。为此，采用三种溶剂的湿法机械力化学法和干法机械力化学合成法制备了PX和SA混合物，并用中、近红外光谱、粉末X射线衍射仪和差示扫描量热仪对其进行了表征。湿法产物的混合物转变为PX/SA 1：1共晶。溶剂的作用是PX与SA共结晶的关键。干燥过程中的产物转变为非晶相。对于非晶态混合物样品，在热分析中观察到两个晶化放热峰。块状PX被研磨相同次数进行转化，但没有成功转化为无定形块体；SA也是如此。认为PX和SA的相互存在促进了相互的非晶化。
The purpose of this study is to investigate the effects of dry and wet mechanochemical synthesis on piroxicam (PX) and saccharin (SA) mixtures. For this purpose, PX and SA mixtures prepared by wet mechanochemical processes using three solvents and by dry mechanochemical synthesis were evaluated by mid-and near-infrared spectroscopy, powder X-ray diffraction (PXRD), and differential scanning calorimetry (DSC). The mixtures of wet-type products were transformed into PX/SA 1:1 co-crystals. The effect of the solvent was key to the co-crystallization of PX and SA. The products from the dry process were transformed into the amorphous phase. For the sample of the amorphous mixture, two exothermic peaks due to crystallization were observed in the thermal analysis. Bulk PX was ground for the same number of times for transformation, but was not successfully transformed to the amorphous bulk; the same was observed for SA. It is suggested that the mutual existence of PX and SA promotes mutual amorphization.