Analysis of chlorthalidone polymorphs in raw materials and tablets and the effect of forms I and II on the dissolution properties of drug products

Bonfílio, Rudy; Leal, Jockastta Silva; Santos, Olimpia Maria Martins; Pereira, Gislaine Ribeiro; Araújo, Magali Benjamim

doi:10.1016/j.jpba.2013.10.020

Cited by 21 publications

(15 citation statements)

References 17 publications

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“…(ii) According to the USP general chapter on X-ray diffraction, the agreement in the 2θ-diffraction angles between specimen and reference is within ±0.2⁰ for the same crystal form, while relative intensities between specimen and reference may vary considerably due to preferred orientation effects 20 .…”

Section: Fig 2: Ftir Spectra Of Solid Forms Of Curcuminoids Curcuminmentioning

confidence: 98%

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2016

IJPSR

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Curcuminoids are dietary phytochemicals obtained from dried rhizomes of turmeric plant (Curcuma longa). Curcuminoids are mixture of curcumin, demethoxy curcumin and bisdemethoxy curcumin in which curcumin is a major constituent. Several polymorphic forms of curcumin were reported. The present study relates to the preparation of different solid forms of curcuminoids and to study the influence of other constituents of curcuminoids on the polymorphic behaviour of curcumin. The developed solid forms were characterized by various spectral methods like Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction (PXRD), Differential Scanning Calorimetry (DSC) and Scanning Electron microscopy (SEM). On crystallization from ethanol and upon melt crystallization, curcuminoids underwent transformation into an amorphous form. Grinding did not affect the polymorphic nature of curcuminoids. These findings suggest that curcuminoids undergo polymorphic modifications very similar to curcumin.

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Section: Fig 2: Ftir Spectra Of Solid Forms Of Curcuminoids Curcuminmentioning

confidence: 98%

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2016

IJPSR

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“…The diffraction pattern is related to the packing of the crystal structure and its array in the solid state (Bonfilio et al, 2014). To determine the occurrence of polymorphisms in APIs of SPR, diffractograms (SPR-L1 to L5, and SPR-pd2º NCQ) were compared to data available from the Cambridge Structural Database (CSD) for crystal form I (Dideberg;Dupont, 1972) and crystal form II (Agafonov, Legendre, Rodier, 1989).…”

Section: Characterization Of Active Pharmaceutical Ingredientsmentioning

confidence: 99%

“…When a pharmaceutical solid exists in more than one form or crystal structure, significant differences in drug solubility may be detected, particularly for drugs that are poorly water-soluble and classified as class II and IV according to the BCS (FDA, 2007;Bonfilio et al, 2014). In these cases, the dissolution step is the limiting step for drug absorption, and the lack of bioequivalence among different formulations may be related to polymorphisms (Amidon et al, 1995;Bauer et al, 2001;Desiraju, 2008;Aaltonen et al, 2009;Babu, Nangia, 2011;Santos et al, 2014;Atici, Karliga, 2015).…”

Section: Introductionmentioning

confidence: 99%

Analysis of spironolactone polymorphs in active pharmaceutical ingredients and their effect on tablet dissolution profiles

Resende

Viana

Freitas

et al. 2016

Braz. J. Pharm. Sci.

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Spironolactone (SPR) is a steroidal drug administered as a potassium-sparing diuretic for high blood pressure treatment. The drug shows incomplete gastrointestinal absorption due to its poor aqueous solubility. The physicochemical properties of SPR in crystal forms I and II suggest that differences in their aqueous solubility may lead to a lack of bioequivalence between solid-state formulations. In this study, SPR polymorphs in five batches of active pharmaceutical ingredients (APIs) from three manufacturers were characterized using powder X-ray diffraction, infrared spectroscopy, thermal analysis, and solubility measurements. SPR tablets (50 mg) were manufactured in our laboratory using API in pure form II, and API in form II contaminated with form I, which was found in a commercial batch. Physicochemical quality evaluations of the manufactured tablets, along with five SPR tablets marketed in Brazil, were performed, and results indicated differences in their dissolution profiles. In the manufactured tablets, differences were associated with the increased solubility of API in form II contaminated with form I compared to API in pure form II. In the marketed SPR tablets, the formulation composition demonstrated an important role in the dissolution rate of the drug, leading to lack of pharmaceutical equivalence among the drug products.Uniterms: Spironolactone/dissolution profile. Spironolactone/pharmaceutical equivalence. Spironolactone/solubility. Spironolactone/polymorphism. Drugs/quality assessment.

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“…X-ray diffractometry is listed as a Category A analytical technique by the Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG). [32] Since different polymorphic forms of the same substance will give different XRD patterns, [33,34] this technique was used to confirm polymorphism in 1 hydrochloride. The two conformations have significantly dissimilar shapes ( Figure 2) and, therefore, the packing of the molecules in each polymorph will not be the same.…”

Section: Powder X-ray Diffraction (Xrd)mentioning

confidence: 99%

Identification of polymorphism in ethylone hydrochloride: synthesis and characterization

Maheux

Alarcon

Copeland

et al. 2015

Drug Testing and Analysis

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Ethylone, a synthetic cathinone with psychoactive properties, is a designer drug which has appeared on the recreational drug market in recent years. Since 2012, illicit shipments of ethylone hydrochloride have been intercepted with increasing frequency at the Canadian border. Analysis has revealed that ethylone hydrochloride exists as two distinct polymorphs. In addition, several minor impurities were detected in some seized exhibits. In this study, the two conformational polymorphs of ethylone hydrochloride have been synthesized and fully characterized by FTIR, FT‐Raman, powder XRD, GC‐MS, ESI‐MS/MS and NMR (13C CPMAS, 1H, 13C). The two polymorphs can be distinguished by vibrational spectroscopy, solid‐state nuclear magnetic resonance spectroscopy and X‐ray diffraction. The FTIR data are applied to the identification of both polymorphs of ethylone hydrochloride (mixed with methylone hydrochloride) in a laboratory submission labelled as 'Ocean Snow Ultra’. The data presented in this study will assist forensic scientists in the differentiation of the two ethylone hydrochloride polymorphs. This report, alongside our recent article on the single crystal X‐ray structure of a second polymorph of this synthetic cathinone, is the first to confirm polymorphism in ethylone hydrochloride. © 2015 Canada Border Services Agency. Drug Testing and Analysis published by John Wiley & Sons, Ltd. © 2015 Canada Border Services Agency. Drug Testing and Analysis published by John Wiley & Sons, Ltd.

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Analysis of chlorthalidone polymorphs in raw materials and tablets and the effect of forms I and II on the dissolution properties of drug products

Cited by 21 publications

References 17 publications

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Analysis of spironolactone polymorphs in active pharmaceutical ingredients and their effect on tablet dissolution profiles

Identification of polymorphism in ethylone hydrochloride: synthesis and characterization

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