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首页> 外文期刊>RSC Advances >Stepwise dissolution and composition determination of samples of multiple crystals using a dissolution medium containing aqueous alcohol and fluorocarbon phases
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Stepwise dissolution and composition determination of samples of multiple crystals using a dissolution medium containing aqueous alcohol and fluorocarbon phases

机译：使用含有含水醇和碳氟化合物相的溶解介质逐步溶解和测定多晶体样品

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摘要

Crystallisations are widely used in pharmaceutical and fine chemical manufacturing to control impurity levels, however crystallisations do not always reduce impurities to acceptable levels. Information on the location and distribution of impurities in crystallised materials would be helpful in such cases. A two phase dissolution medium featuring a fluorocarbon non-solvent vehicle and a aqueous ethanol solvent phase has been used to determine the composition of multi-particle crystalline samples through a partial dissolution approach combined with particle sizing and HPLC analysis. 4-Chloro-2-nitroacetanilide ( 1 ) was chosen as the host compound for this study, with 4-methyl-2-nitroacetanilide ( 2 ) and 4- tert -butyl-2-nitroacetanilide ( 3 ) chosen as the guest impurities that were added to supersaturated toluene solutions of 1 at levels up to 5 mol%. The crystals that formed were subjected to a series of partial dissolution steps carried out using the biphasic dissolution medium composed of a 50% aqueous ethanol solvent phase and a perfluorohexane continuous phase. To inhibit particle agglomeration, the mixture also contained 13,13,14,14,15,15,16,16,17,17,18,18-dodecafluoro-2,5,8,11-tetraoxaoctadecane ( 4 ) as a non-ionic surfactant. The partial dissolution steps showed a relatively even dissolution with each sequential step as determined from particle sizing. Analysis of the solutions by HPLC from each partial dissolution step allowed the level of impurity to be determined, and when combined with the particle sizing data this allowed an impurity distribution to be generated. Impurity 2 was found to be relatively evenly distributed while impurity 3 was localised on or near the surfaces of crystals.
机译：结晶广泛用于制药和精细化工生产中以控制杂质含量，但是结晶并不总是将杂质降低到可接受的水平。在这种情况下，有关结晶材料中杂质的位置和分布的信息将很有帮助。通过部分溶解方法，结合颗粒大小和HPLC分析，已使用具有碳氟化合物非溶剂载体和乙醇水溶液水溶液的两相溶解介质来确定多颗粒晶体样品的组成。选择4-氯-2-硝基乙酰苯胺（1）作为本研究的主体化合物，选择4-甲基-2-硝基乙酰苯胺（2）和4-叔丁基-2-硝基乙酰苯胺（3）作为杂质将其以至多5mol％的水平添加到1的过饱和甲苯溶液中。使用由50％的乙醇溶剂水溶液相和全氟己烷连续相组成的双相溶解介质，对形成的晶体进行一系列的部分溶解步骤。为了抑制颗粒的团聚，混合物还包含13,13,14,14,15,15,16,16,17,17,18,18-十二氟-2,5,8,11-四氧十八碳烷（4）离子表面活性剂。根据颗粒大小确定，每个步骤的部分溶解步骤均显示相对均匀的溶解。通过每个部分溶解步骤的HPLC分析溶液，可以确定杂质含量，当与颗粒尺寸数据结合时，可以生成杂质分布。发现杂质2相对均匀地分布，而杂质3位于晶体表面上或附近。

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