Development of crystallization conditions for obtaining crystalline particles of co-crystals with desired quality

2021 Fiscal Year Final Research Report

• Project/Area Number: 20K15072
• Research Category: Grant-in-Aid for Early-Career Scientists
• Allocation Type: Multi-year Fund
• Review Section: Basic Section 27010:Transport phenomena and unit operations-related
• Research Institution: Tokyo University of Agriculture and Technology
• Principal Investigator: Amari Shuntaro 東京農工大学, 工学(系)研究科(研究院), 助教 (30837737)
• Project Period (FY): 2020-04-01 – 2022-03-31
• Keywords: 多成分結晶 / 包接化合物 / 水和物 / 多成分相図

Outline of Final Research Achievements

The relationship between operation conditions of crystallization and solid phase properties for multicomponent crystal was investigated using cucurbit[7]uril (CB7) which is available for inclusion compound as a model compound.
In the case of CB7 hydrate, which is composed of CB7 and water, we found that the solid phase depends on the temperature and amount of solvent (water) during the crystallization. Furthermore, the solid phase which is precipitated by anti-solvent crystallization was characterized by XRD and DSC. As a result, specific clear peaks derived from the crystal and particle growth were observed when the mixing ratio of anti-solvent was less than 10%, This means that a region where CB7 hydrate was precipitated as the crystalline particles was found on the phase diagram of CB7. These results indicate that crystallization conditions were obtained to produce CB7 hydrate, which is one of the multicomponent crystals, as the crystalline particles.

Free Research Field

晶析

Academic Significance and Societal Importance of the Research Achievements

CB7のように複数の分子から構成される多成分結晶の場合でも、目的成分を含む多成分相図を作成し、結晶化工学の観点から相図に基づいて晶析条件を検討することによって、溶液中から目的の多成分結晶粒子群を安定的に析出させることが可能であることを実験的に示すことができました。また、比較的水に対する溶解性が高いCB7の分離精製に関する知見は、医薬品分野での包接化による有効成分の溶解性改善をはじめとした、CB7を用いた新たな材料創製に関する研究開発に貢献できると考えられます。