Ultrasound assisted cocrystallization from solution (USSC) containing a non-congruently soluble cocrystal component pair: Caffeine/maleic acid
Ultrasound assisted cocrystallization from solution (USSC) containing a non-congruently soluble cocrystal component pair: Caffeine/maleic acid
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DOI：
10.1016/j.ejps.2010.08.012
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发表时间：
2010-12-23
影响因子：
4.6
通讯作者：
York, Peter
中科院分区：
文献类型：
--
作者：
Aher, Suyog;Dhumal, Ravindra;York, Peter
采用超声辅助溶液共结晶法研究了咖啡因和马来酸在甲醇中的非等容溶解对。将USSC与溶剂冷却和浆料超声处理进行比较，使用溶液/浆料中的咖啡因：马来酸（1：0.5、1：1、1：2、1：3和1：3.5）的不同摩尔比。用PXRD和拉曼光谱技术对产物进行了表征。在USSC试验中，观察到产物中共晶的含量随着溶液中马来酸量的增加而增加。当咖啡因与马来酸的摩尔比为1：3.5时，只有USSC得到了纯的咖啡因/马来酸2：1共晶产物。在这两种技术中均未获得咖啡因/马来酸1：1共晶和马来酸。溶剂冷却和浆液超声处理实验的产物是咖啡因和咖啡因/马来酸2：1共晶的不同量的混合物。在USSC中，超声应用必须同时达到溶液中共晶组分的过饱和，这是由于改变的过饱和条件导致共晶形成。对于这种同时达到过饱和，共晶组分在溶液中的摩尔比被确定为一个重要的参数，同时设计实验的非全等可溶对具有大的溶解度差异。(C)2010 Elsevier BV保留所有权利。
Ultrasound assisted solution cocrystallization (USSC) has been studied using a non-congruently soluble pair of caffeine and maleic acid in methanol. USSC was compared with solvent cooling and slurry sonication using different molar ratios of caffeine:maleic acid (1:0.5, 1:1, 1:2, 1:3 and 1:3.5) in solution/slurry. Products were characterized by PXRD and Raman spectroscopy techniques. In USSC trials, the content of cocrystal in the product was observed to increase with increase in amount of maleic acid in solution. Only USSC offered pure caffeine/maleic acid 2:1 cocrystal product when caffeine:maleic acid; 1:3.5 molar ratio was taken in solution. Caffeine/maleic acid 1:1 cocrystal and maleic acid were not obtained in neither of the techniques. Products of solvent cooling and slurry sonication experiments were mixtures of caffeine and caffeine/maleic acid 2:1 cocrystal in varying amounts. In USSC, ultrasound application must have attained simultaneous supersaturation of cocrystal components in solution due to altered supersaturation conditions resulting in cocrystal formation. For this simultaneous attainment of supersaturation, molar ratio of cocrystal components in solution was identified as an important parameter while designing experiments for a non-congruently soluble pair having large solubility difference. (C) 2010 Elsevier B.V. All rights reserved.