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 13mM boric acid and phosphoric acid, adjusted to pH 9.1 with 1M sodium hydroxide, containing 73mM 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.
Micellar electrokinetic chromatography for the simultaneous determination of ketorolac tromethamine and its impurities. Multivariate optimization and validation / S. ORLANDINI; S. FANALI; S. FURLANETTO; A.M. MARRAS; S. PINZAUTI. - In: JOURNAL OF CHROMATOGRAPHY A. - ISSN 0021-9673. - STAMPA. - 1032:(2004), pp. 253-263. [10.1016/j.chroma.2003.08.110]
Micellar electrokinetic chromatography for the simultaneous determination of ketorolac tromethamine and its impurities. Multivariate optimization and validation
ORLANDINI, SERENA;FURLANETTO, SANDRA
;PINZAUTI, SERGIO
2004
Abstract
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 13mM boric acid and phosphoric acid, adjusted to pH 9.1 with 1M sodium hydroxide, containing 73mM 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.File | Dimensione | Formato | |
---|---|---|---|
2004_Orlandini-S._J.-Chromatogr.-A.pdf
Accesso chiuso
Tipologia:
Altro
Licenza:
Tutti i diritti riservati
Dimensione
389.33 kB
Formato
Adobe PDF
|
389.33 kB | Adobe PDF | Richiedi una copia |
I documenti in FLORE sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.