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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 45-60 
    ISSN: 1572-8943
    Keywords: caffeine ; carbamazepine ; crystal forms ; heat of sublimation ; polymorphism ; theophylline ; transition temperature ; vapor pressure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In order to determine the applicability of vapor pressure studies on polymorphic modifications, pairs of enantiotropically related modifications of caffeine, theophylline and carbamazepine were investigated. The studies were performed over a wide temperature range (71 to 191°C) and accordingly over a wide vapor pressure range (0.02 to 400 Pa) using an automatic instrument constructed on the basis of the gas saturation principle. This instrument enables an analytical determination of the main component and the impurities present by the chromatographic separation of the substances transported in the gas flow. Therefore, the real partial pressure of the main component can be measured. Due to the high precision of the applied method it was possible to determine partial pressure curves and the thermodynamic transition temperature — the point at which the vapor pressure of two crystal polymorphs is equal. The thermodynamic transition temperatures of caffeine and theophylline were determined to be 136 and 232°C, respectively. These values are in agreement with experimental or calculated values derived from DSC investigations but are more reliable. Vapor pressure measurements of carbamazepine are only meaningful in the low temperature range due to its decomposition at high temperatures. The thermodynamics, advantages and limits of vapor pressure determinations of polymorphic modifications are discussed.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1572-8943
    Keywords: hot-stage Raman microscopy ; lufenuron CAS RN [103055-07-8] ; paracetamol CAS RN [103-90-2] ; polymorphism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The use of hot-stage Raman microscopy — the direct coupling of Raman spectroscopy and thermomicroscopy — is demonstrated for the drug substances paracetamol and lufenuron. Paracetamol is a well-known analgesic and antipyretic drug, for which three polymorphic forms are currently known. Lufenuron is a benzoylphenyl urea derivative that has been classified as a chitin synthesis inhibitor. It is indicated for the use in pets for the prevention and control of flea population and used in crop protection for the control of Lepidoptera, Western Flower thrips and rust mites. It is the first time that the polymorphism of lufenuron is addressed. All known modifications of paracetamol and lufenuron were produced and identified by hot-stage Raman microscopy. A close correlation of thermal and spectroscopic information was achieved by this combination of techniques. For lufenuron a series of new polymorphic forms were found and characterized. Raman spectroscopy allowed to identify the thermodynamic stable form A as the one which is marketed in tablets.
    Type of Medium: Electronic Resource
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