Identification of Phase Boundaries in Anhydrate/Hydrate Systems

Krzyzaniak, Joseph F.; Williams, Glenn R.; Ni, Nina

doi:10.1002/jps.20941

Cited by 43 publications

(42 citation statements)

References 41 publications

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“…Crystalline polymorph in ethanol/water mixtures Raman spectroscopy Baclofen [127] Solution-mediated hydrate formation to baclofen monohydrate Wet granulation Raman spectroscopy Azithromycin [49] Hydrate formation to azithromycin monohydrate and dihydrate Storage experiments in a desiccator or humidity cell NIR spectroscopy Caffeine [128] Hydrate formation to a non-stoichiometric hydrate of caffeine, dehydrate formation Humidity cell NIR spectroscopy Risedronate sodium [129] Dehydrate formation of risedronate sodium hemi-pentahydrate Fluid-bed drying Raman spectroscopy Theophylline [130] Dehydrate formation of theophylline monohydrate Fluid-bed drying NIR and Raman spectroscopy Carbamazepine, piroxicam [131] Dehydrate formation of carbamazepine dihydrate and piroxicam monohydrate [82,135] Dehydrate formation of piroxicam monohydrate…”

Section: Raman Spectroscopymentioning

confidence: 99%

“…[49] NIR spectroscopy has also been used to study the influence of time, temperature and humidity on interconversions of the anhydrate/hydrate system of caffeine. [128] Phase boundaries at which minimal conversion between the anhydrous and hydrated form of caffeine occurred were identified from the kinetic data. Overall, it was found that quantitative NIR spectroscopy can be used to rapidly determine the stability of solvatomorphs as well as the kinetics of solid-state transformations.…”

Section: Raman Spectroscopymentioning

confidence: 99%

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Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

et al. 2009

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Objectives Solid-state transformations may occur during any stage of pharmaceutical processing and upon storage of a solid dosage form. Early detection and quantification of these transformations during the manufacture of solid dosage forms is important since the physical form of an active pharmaceutical ingredient can significantly influence its processing behaviour, including powder flow and compressibility, and biopharmaceutical properties such as solubility, dissolution rate and bioavailability. Key findings Vibrational spectroscopic techniques such as infrared, near-infrared, Raman and, most recently, terahertz pulsed spectroscopy have become popular for solidstate analysis since they are fast and non-destructive and allow solid-state changes to be probed at the molecular level. In particular, Raman and near-infrared spectroscopy, which require no sample preparation, are now commonly used coupled to fibreoptic probes and are able to characterise solid-state conversions in-line. Traditionally, uni-or bivariate approaches have been used to analyse spectroscopic data sets; however, recently the simultaneous detection of several solid-state forms has been increasingly performed using multivariate approaches where even overlapping spectral bands can be analysed. Summary This review discusses the applications of different vibrational spectroscopic techniques to detect and monitor solid-state transformations possible for crystalline polymorphs, hydrates and amorphous forms of pharmaceutical compounds. In this context, the theoretical basis of solid-state transformations and vibrational spectroscopy and common experimental approaches are described, including recent methods of data analysis.

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Section: Raman Spectroscopymentioning

confidence: 99%

Section: Raman Spectroscopymentioning

confidence: 99%

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

et al. 2009

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“…The thermodynamic stability relationships between anhydrous and hydrated crystal forms are traditionally characterized by the determination of the critical water activity at room temperature (RT), above which the hydrated form is thermodynamically stable. 5,6 The traditional solubility and slurry methods enable accurate determination of the thermodynamic stability relationships for anhydrous polymorphic systems that do not interconvert or transform to hydrates or solvates upon exposure to solvent. However, a solid-state method is required for polymorphic systems that are known to rapidly form hydrates and solvates in the presence of solvents.…”

Section: Introductionmentioning

confidence: 99%

Thermodynamic Stability Considerations for Isostructural Dehydrates

Murphy

Casteel

Samas

et al. 2012

Journal of Pharmaceutical Sciences

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“…The equilibrium water activity of the anhydrous/hydrate system in a slurry experiment has a direct correlation with the equilibrium relative humidity in solid state at the same temperature, because water activity is the ratio of water vapor pressure in a hydrate system to the water vapor pressure of pure water. 7) Water content (8.0%v/v) for the anhydrous to the mono-hydrate form transformation at 25°C corresponds to a water activity of 0.74, 20,21) suggesting that solid state transformation of the anhydrous to the monohydrate form could occur at more than 74% RH.…”

Section: Hydrate Formation Screening By Dvs Measurementmentioning

confidence: 97%

“…6) There are several approaches for investigation of the anhydrous/hydrate phase transformation, such as dynamic water vapor sorption/desorption isotherm (DVS), storage under high humidity, and slurry experiments in water-content-controlled organic solvent mixtures. [7][8][9][10] Cui and Yao explained that slurry experiments using water and organic solvent mixtures under water-content-controlled-conditions were rapid and reliable hydrate screening approaches. 1) Some applications of slurry experiments with water and organic solvent mixtures to investigate the stability in the anhydrous/hydrate system of theophylline and ampicillin, carbamazepine were also reported.…”

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confidence: 99%

Screening and Characterization of Hydrate Forms of T-3256336, a Novel Inhibitor of Apoptosis (IAP) Protein Antagonist

Takeuchi

Kojima

Hashimoto

et al. 2015

CHEMICAL & PHARMACEUTICAL BULLETIN

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Different crystal packing of hydrates from anhydrate crystals leads to different physical properties, such as solubility and stability. Investigation of the potential of varied hydrate formation, and understanding the stability in an anhydrous/hydrate system, are crucial to prevent an undesired transition during the manufacturing process and storage. Only one anhydrous form of T-3256336, a novel inhibitor of apoptosis (IAP) protein antagonist, was discovered during synthesis, and no hydrate form has been identified. In this study, we conducted hydrate screening such as dynamic water vapor sorption/desorption (DVS), and the slurry experiment, and characterized the solid-state properties of anhydrous/hydrate forms to determine the most desirable crystalline form for development. New hydrate forms, both mono-hydrate and hemi-hydrate forms, were discovered as a result of this hydrate screening. The characterization of two new hydrate forms was conducted, and the anhydrous form was determined to be the most desirable development form of T-3256336 in terms of solid-state stability. In addition, the stability of the anhydrous form was investigated using the water content and temperature controlled slurry experiment to obtain the desirable crystal form in the crystallization process. The water content regions of the stable phase of the desired form, the anhydrous form, were identified for the cooling crystallization process. Key words inhibitor of apoptosis (IAP) protein; T-3256336; hydrate; water activityApproximately one-third of pharmaceutical solids have been reported to crystallize in the hydrate forms.1,2) The solidstate characterization of hydrate is essential for pharmaceutical development because the hydrate form has different physicochemical properties such as solubility and stability from its anhydrous form.3-5) Therefore, it is important to discover the possible hydrate forms in early drug development and understand the anhydrous/hydrate phase transformations to ensure undesired conversions do not occur during the development process. 6)There are several approaches for investigation of the anhydrous/hydrate phase transformation, such as dynamic water vapor sorption/desorption isotherm (DVS), storage under high humidity, and slurry experiments in water-content-controlled organic solvent mixtures.7-10) Cui and Yao explained that slurry experiments using water and organic solvent mixtures under water-content-controlled-conditions were rapid and reliable hydrate screening approaches.1) Some applications of slurry experiments with water and organic solvent mixtures to investigate the stability in the anhydrous/hydrate system of theophylline and ampicillin, carbamazepine were also reported.11-13) Water content is related to water activity, defined by the activity coefficient and mole fraction of water.Hydrate formation is represented by the following equilibrium (Eq. 1), previously described by Grant and Higuchi ) in a water and organic solvent mixture is a crucial factor for the hydrate formation. The stability o...

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Identification of Phase Boundaries in Anhydrate/Hydrate Systems

Cited by 43 publications

References 41 publications

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Thermodynamic Stability Considerations for Isostructural Dehydrates

Screening and Characterization of Hydrate Forms of T-3256336, a Novel Inhibitor of Apoptosis (IAP) Protein Antagonist

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