Solid-state evaluation and polymorphic quantification of venlafaxine hydrochloride raw materials using the Rietveld method

TALANTA

卷:117

Article

Bernardi, Larissa S.¹  Ferreira, Fabio F.²  Cuffini, Silvia L.¹  Campos, Carlos E. M.³  Monti, Gustavo A.⁴  Kuminek, Gislaine¹  Oliveira, Paulo R.⁵  Cardoso, Simone G.¹ 

[1] Univ Fed Santa Catarina, Ctr Ciencias Saude, Programa Posgrad Farm, BR-88040900 Florianopolis, SC, Brazil

[2] Univ Fed ABC, Ctr Ciencias Nat & Humanas, Sao Paulo, Brazil

[3] Univ Fed Santa Catarina, Programa Posgrad Fis, BR-88040900 Florianopolis, SC, Brazil

[4] Univ Nacl Cordoba, FAMAF, IFEG CONICET, RA-5000 Cordoba, Argentina

[5] Univ Estadual Ctr Oeste UNICENTRO, Programa Posgrad Ciencias Farmaceut, Guarapuava, PR, Brazil

关键词: Venlafaxine hydrochloride;    Polymorphism;    X-ray powder diffraction;    Rietveld method;   

DOI  :  10.1016/j.talanta.2013.09.006

来源: Elsevier

【 摘 要 】

Venlafaxine hydrochloride (VEN) is an antidepressant drug widely used for the treatment of depression. The purpose of this study was to carry out the preparation and solid state characterization of the pure polymorphs (Forms 1 and 2) and the polymorphic identification and quantification of four commercially-available VEN raw materials. These two polymorphic forms were obtained from different crystallization methods and characterized by X-ray Powder Diffraction (XRPD), Diffuse Reflectance Infrared Fourier Transform (DRIFT), Raman Spectroscopy (RS), liquid and solid state Nuclear Magnetic Resonance (NMR and ssNMR) spectroscopies, Differential Scanning Calorimetry (DSC), and Scanning Electron Microscopy (SEM) techniques. The main differences were observed by DSC and XRPD and the latter was chosen as the standard technique for the identification and quantification studies in combination with the Rietveld method for the commercial raw materials (VEN1-VEN4) acquired from different manufacturers. Additionally Form 1 and Form 2 can be clearly distinguished from their C-13 ssNMR spectra. Through the analysis, it was possible to conclude that VEN1 and VEN2 were composed only of Form 1, while VEN3 and VEN4 were a mixture of Forms 1 and 2. Additionally, the Rietveld refinement was successfully applied to quantify the polymorphic ratio for VEN3 and VEN4. (C) 2013 Elsevier B.V. All rights reserved.

【 授权许可】

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