粉末衍射
材料科学
无水的
无定形固体
结晶
再结晶(地质)
差示扫描量热法
喷雾干燥
结晶度
化学
分析化学(期刊)
结晶学
核化学
色谱法
有机化学
热力学
古生物学
物理
生物
作者
Orsolya Jójárt-Laczkovich,Gábor Katona,Zoltán Aigner,Piroska Szabó‐Révész
标识
DOI:10.1016/j.ejps.2016.08.003
摘要
The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60 °C up to 45% RH and at 70 °C up to 30% RH into dihydrate form. At 70 °C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28 days stored samples the dihydrate form was detected at 40 °C, 50% RH. Storage at 60 °C, 40% RH resulted in the appearance of the anhydrous form and at 60 °C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample.
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