Investigation of polymorphic transitions of piracetam induced during wet granulation

Potter, Catherine B.; Kollamaram, Gayathri; Żegliński, Jacek; Whitaker, Darren; Croker, Denise M.; Walker, Gavin

doi:10.1016/j.ejpb.2017.05.012

Cited by 11 publications

(6 citation statements)

References 27 publications

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“…DSC thermograms obtained for the three solid phases (Form II, Form III, and Form VI; shown in Figure S4 of the Supporting Information) exhibit qualitatively similar behavior; a weak endothermic transformation peak with an onset between 390 and 400 K, followed by a melting peak with an onset at around 426 K, corresponding to the reported melting point of Form I. 20,27 The estimated solubility of Form VI in ethanol and isopropanol at 288.15 K is summarized in Table 3. In mole fraction terms, the estimated solubility is higher in ethanol than in isopropanol, in agreement with data reported for Form II 19 and Form III.…”

Section: Methodsmentioning

confidence: 83%

“…Various analytical techniques like powder X-ray diffraction (PXRD), in situ energy dispersive X-ray diffraction, in situ Raman spectroscopy, infrared spectroscopy (IR), and near-infrared spectroscopy have been used to investigate the solid-state, solution-mediated, and wet granulation-induced polymorphic transformations of piracetam. ,,− Recently, our group published a detailed study on the crystal growth kinetics of the metastable Form II and the stable Form III in two organic solvents . However, to the best of our knowledge, no crystal nucleation induction time study of piracetam has been reported so far .…”

Section: Introductionmentioning

confidence: 99%

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Characterization and Crystal Nucleation Kinetics of a New Metastable Polymorph of Piracetam in Alcoholic Solvents

Kakkar

Zeng

Svärd

et al. 2022

Crystal Growth & Design

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A new polymorph of the drug active pharmaceutical ingredient piracetam (Form VI) has been discovered and characterized by X-ray powder diffraction (PXRD), solid-state Raman, attenuated total reflectance infrared spectroscopy, and differential scanning calorimetry. The PXRD diffractogram of Form VI shows a distinct peak at 24.2°(2θ) that distinguishes it from the previously known polymorphs and solvates. Form VI is metastable with respect to the previously known polymorphs Form II and Form III; in ethanol solution at 288 K, Form VI transforms into Form II within 15 min, while in isopropanol solution Form VI is kinetically stable for at least 6 h. A total of 1200 crystal nucleation induction time experiments of piracetam in ethanol and isopropanol solutions have been conducted, in sets of 40−80 repeat experiments carried out at different temperatures and solute concentrations. Each solution nucleated as a single polymorph, and each set of repeat experiments resulted in different proportions of Form II, Form III, and Form VI, with Form VI dominating at low nucleation temperatures and Form II at higher nucleation temperatures. The induction time data for Form VI at 288 K have been evaluated within the framework of the classical nucleation theory. At equal driving force, nucleation of Form VI is less obstructed in ethanol than in isopropanol, as captured by a lower interfacial energy and higher preexponential factor in ethanol. The proportion of Form VI obtained at a comparable driving force increases in the order ethanol < isopropanol.

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Section: Methodsmentioning

confidence: 83%

Section: Introductionmentioning

confidence: 99%

Characterization and Crystal Nucleation Kinetics of a New Metastable Polymorph of Piracetam in Alcoholic Solvents

Kakkar

Zeng

Svärd

et al. 2022

Crystal Growth & Design

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“…The solubility of FII and FIII forms and their stability have been determined in a range of organic solvents. , These two polymorphs constitute a monotropic system in the range 278–323 K, viz., their solubility curves do not cross. The solid state, solution mediated, , and wet granulation induced polymorphic transformations of PCM have been investigated using various analytical techniques like in situ Raman spectroscopy, infrared spectroscopy (IR), powder X-ray diffraction (PXRD), and near-infrared spectroscopy. , The metastable zone width of PCM in ethanol has been studied as well as the formation of PCM cocrystals with hydroxyl group functionalized carboxylic acids . To the best of our knowledge, there is scant information on crystal growth kinetics of polymorphic systems in general , and no determination whatsoever of the crystal growth behavior of PCM polymorphs.…”

Section: Introductionmentioning

confidence: 99%

“…3,15 These two polymorphs constitute a monotropic system in the range 278− 323 K, viz., their solubility curves do not cross. The solid state, 14 solution mediated, 16,17 and wet granulation induced 18 polymorphic transformations of PCM have been investigated using various analytical techniques like in situ Raman spectroscopy, infrared spectroscopy (IR), powder X-ray diffraction (PXRD), and near-infrared spectroscopy. 13,19 The metastable zone width of PCM in ethanol has been studied 19 as well as the formation of PCM cocrystals with hydroxyl group functionalized carboxylic acids.…”

Section: Introductionmentioning

confidence: 99%

Crystal Growth Kinetics of Piracetam Polymorphs in Ethanol and Isopropanol

Rasmuson

2019

Crystal Growth & Design

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The crystal growth kinetics of two different polymorphs of Piracetam have been investigated in ethanol and isopropanol. Isothermal seeded desupersaturation experiments were carried out at supersaturation ratios below 1.2 within the range of temperature 283–308 K. Liquid concentration was determined by in situ ATR-FTIR spectroscopy by a calibration-free method using principal component analysis. The power law equation and the BCF and B+S models were fitted to the experimental desupersaturation data by nonlinear optimization. The growth rates ranged 10–7–10–8 m/s, the growth rate order is clearly higher than unity, and the activation energies are in the range 39–66 kJ/mol for all the systems studied suggesting surface integration control. The growth of the metastable polymorph is faster than that of the stable form in both solvents. The crystal growth proceeds faster in ethanol than in isopropanol for both polymorphs. The solid–liquid interfacial energy is lower for the metastable form and is for both forms lower in ethanol than in isopropanol. The surface diffusion mass transfer rate is higher for the metastable form compared to the stable form and higher in ethanol than in isopropanol.

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“…It is desirable to be able to automatically identify, reduce and/or remove these spikes from Raman spectra. This becomes even more relevant when processing large mapping datasets prevalent within pharmaceutical research 4,5,6,7 . Methodologies reported in the literature can be broadly separated into three categories: (i) additional acquisition based methods; (ii) methods involving hardware modification; and the category the present work falls into (iii) single-scan correction via filtering or smoothing.…”

Section: Introductionmentioning

confidence: 99%