RESUMO
The paper proposes a near infrared method able to directly and simultaneously quantify ascorbic acid and sodium ascorbate in powder blends for tableting and in vitamin C chewable tablets without any sample preparation. In the first step, calibration models for the quantification of ascorbic acid and sodium ascorbate in powder blends for tableting and subsequently in chewable vitamin C tablets (corresponding to 80-120 % active substance) were developed according to an experimental design with 2 variables and 5 levels. Then, using the best calibration models, the methods were fully validated in terms of recovery, precision and accuracy for both powder blends and vitamin C chewable tablets. The validated concentration range was 15.14-18.51 % for ascorbic acid and 12.06-14.49 % for sodium ascorbate in powder blends and 91.85-111.03 mg per tablet for ascorbic acid and 71.01-84.50 mg per tablet for sodium ascorbate in tablets. Validation results showed good precision and accuracy.
Assuntos
Ácido Ascórbico/química , Mastigação , Espectroscopia de Luz Próxima ao Infravermelho/métodos , Administração Oral , Ácido Ascórbico/administração & dosagem , Química Farmacêutica , Pós , ComprimidosRESUMO
This paper describes the development and application of NIR-chemometric methods for active content assay and pharmaceutical characterization (granulometric analysis and flowability assessment) of indapamide powder blends for tabletting. Indapamide powder blends were prepared and their NIR spectra were recorded in reflectance mode. Partial least-squares (PLS) regression followed by leave-one-out cross-validation was used to develop calibration models for predicting the indapamide content and pharmaceutical properties. The method for indapamide assay was validated in terms of trueness, precision, accuracy. The near infrared based property predictions were compared with the reference method results and no significant differences were found between the reference and predicted characteristics. The developed NIR-chemometric methods can be useful tools for prediction of active content, granulometric properties and parameters related to flowability of pharmaceutical powders.
Assuntos
Anti-Hipertensivos/análise , Diuréticos/análise , Ensaios de Triagem em Larga Escala , Indapamida/análise , Espectroscopia de Luz Próxima ao Infravermelho , Tecnologia Farmacêutica/métodos , Calibragem , Química Farmacêutica , Ensaios de Triagem em Larga Escala/normas , Análise dos Mínimos Quadrados , Análise Multivariada , Tamanho da Partícula , Pós , Controle de Qualidade , Padrões de Referência , Reprodutibilidade dos Testes , Reologia , Espectroscopia de Luz Próxima ao Infravermelho/normas , Comprimidos , Tecnologia Farmacêutica/normasRESUMO
A near infrared (NIR) method able to directly quantify the active content in pharmaceutical powder blends used for manufacturing meloxicam tablets, without any sample preparation, was developed and fully validated. To develop calibration models for the assay of meloxicam in powder blends for tableting, the NIR reflectance spectra of different meloxicam powder blends prepared according to a calibration protocol was analysed using different preprocessing methods by partial last-square regression (PLS) and principal component regression (PCR).The best calibration model was found when partial last-square regression (PLS) was used as regression algorithm in association with Smoothing-Savitsky as pre-processing spectrum method. The trueness, precision (repeatability and intermediate precision), accuracy, linearity and range of application of the developed NIR method were validated according to the International Conference of Harmonization (ICH) and Medicine European Agency (EMA) guidelines and found to be fit for its intended purpose.
