Micellar electrokinetic chromatography for the simultaneous determination of ketorolac tromethamine and its impurities: Multivariate optimization and validation

A simple, fast and selective micellar electrokinetic chromatographic (MEKC) method for the simultaneous assay of ketorolac tromethamine and its known related impurities (1-hydroxy analog of ketorolac, 1-keto analog of ketorolac and decarboxylated ketorolac), in both drug substance and coated tablets...

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Bibliographic Details
Published in:Journal of Chromatography A 2004-04, Vol.1032 (1), p.253-263
Main Authors: Orlandini, S., Fanali, S., Furlanetto, S., Marras, A.M., Pinzauti, S.
Format: Article
Language:English
Subjects:
Analysis
Anti-Inflammatory Agents, Non-Steroidal - analysis
Biological and medical sciences
Calibration
Chromatography, Micellar Electrokinetic Capillary - methods
Experimental design
General pharmacology
Ketorolac tromethamine
Ketorolac Tromethamine - analysis
Medical sciences
Multivariate Analysis
Nonsteroidal anti-inflammatory drugs
Optimization
Pharmaceutical analysis
Pharmacology. Drug treatments
Sensitivity and Specificity
Validation
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Description
Summary:A simple, fast and selective micellar electrokinetic chromatographic (MEKC) method for the simultaneous assay of ketorolac tromethamine and its known related impurities (1-hydroxy analog of ketorolac, 1-keto analog of ketorolac and decarboxylated ketorolac), in both drug substance and coated tablets, is described. The compounds were detected at 323 nm, and flufenamic acid (FL) and tolmetin (TL) were chosen as internal standards to quantify ketorolac tromethamine and impurities, respectively. The multivariate optimization of the experimental conditions was carried out by means of the response surface study, considering as responses the resolution values and analysis time. The optimized background electrolyte (BGE) consisted of a mixture of 13 mM boric acid and phosphoric acid, adjusted to pH 9.1 with 1 M sodium hydroxide, containing 73 mM sodium dodecyl sulfate (SDS). Optimal temperature and voltage were 30 °C and 27 kV. Applying these conditions, all compounds were resolved in about 6 min. The related substances could be quantified up to the 0.1% (w/w) level. Validation was performed, either for drug substances and drug product, evaluating selectivity, robustness, linearity and range, precision, accuracy, detection and quantitation limits and system suitability.
ISSN:0021-9673
DOI:10.1016/j.chroma.2003.08.110