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Acevska J.,Ss. Cyril and Methodius University of Skopje | Stefkov G.,Ss. Cyril and Methodius University of Skopje | Poceva Panovska A.,Ss. Cyril and Methodius University of Skopje | Micovski I.,Production of Pharmaceutical Raw Materials | And 2 more authors.
Journal of Thermal Analysis and Calorimetry | Year: 2016

Important narcotic analgesic active pharmaceutical ingredients (APIs): morphine hydrochloride (MoH), morphine sulfate (MoS) and the starting substance for their semi-synthesis morphine base (MoB), have been characterized by thermoanalytical methods (DSC and TG/DTG) and Fourier transform infrared spectroscopy (FTIR). Additionally, a set of different pattern recognition techniques were used to reveal the differentiation features of the morphine fingerprints obtained from 28 API samples (6 MoS, 9 MoH and 13 MoB) from known origin in order to build a predictive model for authentication of samples of unknown composition. It was observed that important parameters for building pattern recognition model using thermoanalytical data are the same analytical information significant for structural characterization: melting point (observed on DSC curves) and thermal degradation point (observed on TG curves). Hierarchical cluster analysis (HCA), based on these reproducible features, allowed identification of the different MoB and MoS samples origin. However, due to the absence of the characteristic endothermic phenomenon originating from the melting of MoH samples, the required characteristic fingerprinting features were not obtained. The FTIR-ATR spectroscopy study clearly confirmed that the different morphine entities can be easily identified by their infrared signature when spectra are collected without sample preparation in order to preserve the original information about the corresponding molecular structures. However, FTIR analysis showed low discriminatory power for authenticity check of morphine and its derivatives with respect to their different origins, but proved inevitable to detect the 'genuine' falsification. © 2016 Akadémiai Kiadó, Budapest, Hungary.

Micovski I.,Production of Pharmaceutical Raw Materials | Bogoeva-Gaceva G.,Ss. Cyril and Methodius University of Skopje | Jovanovski G.,Macedonian Academy of science and Arts | Jovanovski G.,Ss. Cyril and Methodius University of Skopje | Makreski P.,Ss. Cyril and Methodius University of Skopje
Vibrational Spectroscopy | Year: 2012

The detailed solvatomorphism study of codeine phosphate sesquihydrate - an important narcotic analgesic and antitusic active pharmaceutical ingredient (API) is reported. The extensive crystallization from a series of medium to high polarity solvents clearly exhibited the low affinity toward solvates building of this compound. The materials obtained after crystallization were investigated by vibrational spectroscopy (infrared and Raman) and thermoanalytical methods (DSC and TG/DTG). It was observed that after absolute ethanol, ethyl acetate, acetone and acetonitrile crystallization, direct solvent mediated phase transition of codeine phosphate sesquihydrate to anhydrous codeine phosphate was achieved. When N,N-dimethylformamide was used as crystallization medium, transformation to the hemihydrate form of codeine phosphate was induced. Only in the case of methanol solution, formation of mixed hydrate-methanolate solvate was observed. Compared to the commercial forms of codeine phosphate hydrates, according to the obtained spectroscopic and thermoanalytical data, the newly obtained compound has different molecular arrangement. Based on the data obtained from thermal analysis and water content study, tentative stoichiometry was established and the compound was labeled as codeine phosphate sesquihydrate methanolate. The X-ray powder diffraction (XRPD) measurements confirmed the spectroscopic and thermoanalytical findings about the existence of different crystal structures between the various obtained codeine phosphate solid forms. © 2012 Elsevier B.V. All rights reserved.

Zbacnik M.,University of Zagreb | Trimceski V.,Production of Pharmaceutical Raw Materials | Kaitner B.,University of Zagreb | Jovanovski G.,Macedonian Academy of science and Arts | And 2 more authors.
Journal of Crystal Growth | Year: 2013

The first crystal structure elucidation of pholcodine monohydrate, an important antitussive active pharmaceutical ingredient is reported herein. The studied compound crystallizes in the orthorhombic system in the space group P212121. Each H2O molecule is shared by two pholcodine molecules via three strong hydrogen bonds. The detailed crystallization screening from several different organic solvents afforded single crystals with various quality, all exhibiting prism-to-needlelike micro morphology. The investigation of the obtained single crystals by means of several physico-chemical, solid-state instrumental techniques (FT-IR, DSC, TG/DTG and XRPD) proved that pholcodine monohydrate exists in a single crystalline modification, identical to the commercial form of the compound. © 2013 Elsevier B.V.

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