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    Pharmaceutical Co-crystals. Combining thermal microscopy and phase space considerations to facilitate the growth of novel phases.

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    Publication date
    2011-07-06
    Author
    Berry, David J.
    Supervisor
    Blagden, Nicholas
    Storey, Richard
    Keyword
    Pharmaceutical
    Co-crystals
    Design
    Thermal
    Microscopy
    Screening
    Nicotinamide
    Ibuprofen
    Crystal engineering
    Rights
    Creative Commons License
    The University of Bradford theses are licenced under a Creative Commons Licence.
    Institution
    University of Bradford
    Department
    School of pharmacy
    Awarded
    2009
    
    Metadata
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    Abstract
    The crystalline solid state is invaluable to both the pharmaceutical and fine chemical sectors. The advantages primarily relate to reducibility criteria required during processing of stable solid state materials and delivering purification, which is inherently performed by the crystal growth process. A major challenge is achieving control through crystallising solids with the desired physico-chemical properties. If this can be achieved the crystalline solid is of great financial and practical benefit. One emerging methodology for manipulating the solid crystalline form is the application of co-crystals. This work relates to key steps in the understanding of rational design of co-crystals utilizing crystal engineering concepts to determine systems before then applying screening criteria to the selected sub-set. Co-crystal screening is routinely undertaken using high-throughput solution growth. We report a low- to medium-throughput approach, encompassing both a melt and solution crystallization step as a route to the identification of co-crystals. Prior to solution studies, a melt growth step was included utilizing the Kofler mixed fusion method. This method allowed elucidation of the thermodynamic landscape within the binary phase diagram and was found to increase overall screening efficiency. This led to the discovery of a number of co-crystal systems with the co-former nicotinamide, with the single crystal structures determined for the following systems; R/S ibuprofen: nicotinamide, S ibuprofen: nicotinamide, R/S flurbiprofen: nicotinamide and salicylic acid: nicotinamide. To assess the crystallization and phase behaviours of determined co-crystals the R/S ibuprofennicotinamide system was selected and successful studies were undertaken determining the aqueous ternary phase behavior and the pre-nucleation speciation in methanol. There have, as yet, been a limited number of published examples which are concerned with pharmaceutical property enhancement by co-crystals, as vast proportion of the literature concerns the growth and isolation of these novel phases. To elucidate further the pharmaceutical relevance of co-crystals the properties of the R/S ibuprofen- nicotinamide system were then assessed showing a positive profile for this material.
    URI
    http://hdl.handle.net/10454/4932
    Type
    Thesis
    Qualification name
    PhD
    Notes
    The accompanying "Experimental raw data files and cifs" are not available online.
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