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J Pharm Biomed Anal ; 70: 652-6, 2012 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-22884784

RESUMO

This study aimed to develop and validate a stability indicating LC for the determination of 5-(2-benzoylethenyl)-N-benzyl-2 methoxybenzenesulfonamide (SCD - a synthetic chalcone derivative), and evaluate the degradation profile of the compound under different stress conditions recommended by International Conference on Harmonization (ICH). Chromatographic separation was performed on a silica C18 column, methanol-water mobile phase 70:30 (v:v), pH 5.0 adjusted with the addition of trifluoroacetic acid (TFA) at a flow rate of 1.0 mL min(-1); detection by UV absorption at 330 nm. The method was validated for linearity, precision, accuracy, robustness and specificity. The SCD was subjected to forced degradation and peak photodegradation product was well separated from the pure substance, with retention times significantly different, indicating the specificity of the method. Second-order degradation kinetics of SCD was observed under photodegradation and base-induced degradation. In order to identify the product formed under photodegradation, liquid chromatography-tandem mass spectrometry (LC-MS/MS) was performed. These results indicate that the method can be successfully used in order to assay SCD in a nanoemulsion dosage form, and that this formulation has a protective effect over SCD degradation.


Assuntos
Chalcona/análise , Cromatografia Líquida de Alta Pressão , Nanopartículas , Fotólise , Espectrometria de Massas por Ionização por Electrospray , Calibragem , Chalcona/análogos & derivados , Chalcona/síntese química , Chalcona/efeitos da radiação , Cromatografia Líquida de Alta Pressão/normas , Formas de Dosagem , Estabilidade de Medicamentos , Emulsões , Cinética , Modelos Lineares , Metanol/química , Nanotecnologia , Padrões de Referência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Dióxido de Silício/química , Espectrometria de Massas por Ionização por Electrospray/normas , Espectrofotometria Ultravioleta , Ácido Trifluoracético/química , Raios Ultravioleta , Água/química
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