Characterizing the conversion kinetics of carbamazepine polymorphs to the dihydrate in aqueous suspension using Raman spectroscopy

Tian, Fang; Zeitler, J. Axel; Strachan, Clare J.; Saville, Dorothy J.; Gordon, Keith C.; Rades, Thomas

doi:10.1016/j.jpba.2005.07.030

Cited by 97 publications

(71 citation statements)

References 47 publications

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“…Powder dissolution of carbamazepine at pH 2 reached 185 μg/ mL before precipitating after 77 min. The precipitation event probably represents transformation to the less soluble dihydrate form (26). The powder of the CBZ-SAC cocrystal had a faster initial dissolution rate than the CBZ powder although the peak concentration was the same (186 μg/mL) and precipitation was observed at a much earlier time point (11 min).…”

Section: Discussionmentioning

confidence: 99%

“…The samples continued to dissolve reaching peak concentrations of 197±47 μg for CBZ-NIC after 2 min, 371±24 μg for CBZ-SAC after 11 min and 370±5 μg after 77 min for pure CBZ. The drop in concentration observed following dissolution of the pure CBZ is probably due to the formation of the less soluble carbamazepine dihydrate form (26). The concentration decreased to 285±7 μg of dissolved carbamazepine by the end of the 4-h experiment.…”

Section: Carbamazepine (Cbz) and Its Cocrystals (Cbz-sac Cbz-nic)mentioning

confidence: 92%

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Small-Scale Assays for Studying Dissolution of Pharmaceutical Cocrystals for Oral Administration

et al. 2015

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Abstract. The purpose of this study was to better understand the dissolution properties and precipitation behavior of pharmaceutical cocrystals of poorly soluble drugs for the potential for oral administration based on a small-scale dissolution assay. Carbamazepine and indomethacin cocrystals with saccharin and nicotinamide as coformers were prepared with the sonic slurry method. Dissolution of the poorly soluble drugs indomethacin and carbamazepine and their cocrystals was studied with a small-scale dissolution assay installed on a SiriusT3 instrument. Two methodologies were used: (i) surface dissolution of pressed tablet (3 mm) in 20 mL running for fixed times at four pH stages (pH 1.8, pH 3.9, pH 5.4, pH 7.3) and (ii) powder dissolution (2.6 mg) in 2 mL at a constant pH (pH 2). Improved dissolution and useful insights into precipitation kinetics of poorly soluble compounds from the cocrystal form can be revealed by the smallscale dissolution assay. A clear difference in dissolution/precipitation behaviour can be observed based on the characteristics of the coformer used.

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Section: Discussionmentioning

confidence: 99%

Section: Carbamazepine (Cbz) and Its Cocrystals (Cbz-sac Cbz-nic)mentioning

confidence: 92%

Small-Scale Assays for Studying Dissolution of Pharmaceutical Cocrystals for Oral Administration

et al. 2015

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“…Humidity cell Raman spectroscopy Carbamazepine [125,126] Solution-mediated hydrate formation to carbamazepine dihydrate…”

Section: Solvatesmentioning

confidence: 99%

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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“…the primitive monoclinic polymorph (form I), trigonal polymorph (form II) and triclinic polymorph (form III)) and dihydrate (form IV) have been well characterized by XRD, DSC, 13 C-NMR, FT-IR, and Raman spectroscopy. [21][22][23][24][25] The polymorphic content of pharmaceuticals is determined and predicted by the XRD method, but this method has relatively large errors, of around ±5%, due to the crystal orientation when the sample powder is loaded on the glass plate. If these problems are solved, the X-ray diffraction method might be applicable to on-line pharmaceutical manufacturing processes as a non-destructive measurement method.…”

Section: Analytical Sciences April 2008 Vol 24mentioning

confidence: 99%

An Accurate Quantitative Analysis of Polymorphic Content by Chemometric X-ray Powder Diffraction

2008

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Data from X-ray powder diffraction (XRD) were subjected to a partial least-squares regression analysis (PLS) to build a calibration model for predicting the polymorphic content of carbamazepine (CBZ). The effectiveness of the PLS method in the construction of calibration models was analyzed by a scientific approach based on a regulation vector. CBZ forms I and III were characterized by differential scanning calorimetry (DSC) and XRD. Powder mixtures of forms I and III at various ratios (0 -100% w/w; form III) were subjected to XRD. Five diffraction peaks were used for the peak-area method to compare with PLS. The results obtained by PLS had a better predictive accuracy compared to those of the peak-area method. The XRD-PLS method was established as a non-destructive, non-contact way to avoid the particle orientation effect based on statistical theory.

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Characterizing the conversion kinetics of carbamazepine polymorphs to the dihydrate in aqueous suspension using Raman spectroscopy

Cited by 97 publications

References 47 publications

Small-Scale Assays for Studying Dissolution of Pharmaceutical Cocrystals for Oral Administration

Small-Scale Assays for Studying Dissolution of Pharmaceutical Cocrystals for Oral Administration

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

An Accurate Quantitative Analysis of Polymorphic Content by Chemometric X-ray Powder Diffraction

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