• 主题
高级搜索  >
历史搜索 清空历史
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
【24h】

Stepwise dissolution and composition determination of samples of multiple crystals using a dissolution medium containing aqueous alcohol and fluorocarbon phases

机译：使用含水醇和氟碳相的溶解介质逐步溶解和组合物测定多晶体的样品

获取原文
获取原文并翻译 | 示例
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

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：结晶广泛用于药物和细化学制造中以控制杂质水平，但是结晶并不总是将杂质减少到可接受的水平。关于结晶材料中杂质的位置和分布的信息在这种情况下会有所帮助。已经使用具有氟碳非溶剂载体和乙醇水溶液水溶液的两相溶解介质来通过部分溶解方法与颗粒尺寸和HPLC分析结合使用颗粒溶解方法来确定多颗粒晶体样品的组成。选择4-氯-2-硝基丙基丙酮（1）作为本研究的宿主化合物，用4-甲基-2-硝基丙酸丁酸乙酯（2）和4-叔丁基-2-硝基丙酸酯（3）作为客体杂质在高达5mol％的水平下加入到过饱和甲苯溶液中。使用由50％乙醇水溶液和全氟己烷连续相组成的双相溶解介质进行形成的晶体进行一系列部分溶出步骤。为了抑制颗粒附聚，该混合物还含有13,13,14,15,15,16,16,17,17,18,18,11-十二烷氟-2,5,8,11-四氧结癸烷（4），为非离子表面活性剂。部分溶出步骤显示出从颗粒尺寸确定的每个顺序步骤的均匀溶解。通过HPLC从每个部分溶解步骤分析溶液允许确定杂质的水平，并且当与颗粒尺寸数据组合时，这允许产生杂质分布。发现杂质2相对均匀地分布，而杂质3在晶体表面上或附近局部地定位。

著录项

  • 来源
    《RSC Advances》 |2019年第37期|共13页
  • 作者

    Moynihan Humphrey A.; Armstrong Declan;

  • 作者单位

    Univ Coll Cork Sch Chem Analyt &

    Biol Chem Res Facil Synth &

    Solid State Pharmaceut Ctr Coll Rd Cork T12 K8AF Ireland;

    Univ Coll Cork Sch Chem Analyt &

    Biol Chem Res Facil Synth &

    Solid State Pharmaceut Ctr Coll Rd Cork T12 K8AF Ireland;

  • 收录信息
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
  • 关键词

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号