Developing and optimizing a validated isocratic reversed-phase high-performance liquid chromatography separation of nimodipine and impurities in tablets using experimental design methodology
| Autor: | Panagiotis Barmpalexis, Emanouil Georgarakis, Feras Imad Kanaze |
|---|---|
| Rok vydání: | 2009 |
| Předmět: |
Time Factors
Central composite design Chemistry Pharmaceutical Clinical Biochemistry Analytical chemistry Pharmaceutical Science Sensitivity and Specificity High-performance liquid chromatography Dosage form Analytical Chemistry Impurity Spectrophotometry Phase (matter) Drug Discovery medicine Chromatography High Pressure Liquid Spectroscopy Chromatography Molecular Structure medicine.diagnostic_test Chemistry Reproducibility of Results Reversed-phase chromatography Factorial experiment Hydrogen-Ion Concentration Reference Standards Calcium Channel Blockers Solutions Pharmaceutical Preparations Nimodipine Spectrophotometry Ultraviolet Drug Contamination Tablets |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 49:1192-1202 |
| ISSN: | 0731-7085 |
| DOI: | 10.1016/j.jpba.2009.03.003 |
| Popis: | In the present study an isocratic reversed-phase high-performance liquid chromatography was investigated for the separation of nimodipine and impurities (A, B and C) using statistical experimental design. Initially, a full factorial design was used in order to screen five independent factors: type of the organic modifier - methanol or acetonitrile - and concentration, column temperature, mobile phase flow rate and pH. Except pH, the rest examined factors were identified as significant, using ANOVA analysis. The optimum conditions of separation (optimum values of significant factors) determined with the aid of central composite design were: (1) mobile phase: acetonitrile/H(2)O (67.5/32.5, v/v), (2) column temperature 40 degrees C and (3) mobile phase flow rate 0.9 ml/min. The proposed method showed good prediction ability (observed-predicted correlation). The analysis was found to be linear, specific, precise, sensitive and accurate. The method was also studied for robustness and intermediate precision using experimental design methodology. Three commercially available nimodipine tablets were analyzed showing good % recovery and %RSD. No traceable amounts of impurities were found in all products. |
| Databáze: | OpenAIRE |
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