| Popis: |
Two simple, accurate, precise, inexpensive, selective and sensitive spectrophotometric methods are described for the determination of repaglinide (RPG) in bulk drug and its tablets. The methods were based on the charge- transfer complex reaction between RPG in acetonitrile with p-chloranilic acid (CAA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in dioxane and subsequent formation of intensely colored radical anions of the reagents which were measured at 520 nm (CAA) or 590 nm (DDQ). Several experimental variables affecting the complex formation, stability of the colored species and sensitivity of the reaction were optimized. Under the optimized conditions, Beer’s law was obeyed over the concentration ranges of 20-400 and 5-80 μg ml-1 RPG for CAA and DDQ methods, respectively, and the corresponding correlation coefficients were 0.9995 and 0.9998. The apparent molar absorptivity values were 1.02x103 and 4.60x103 for CAA and DDQ methods respectively, with corresponding Sandell sensitivity values of 0.4438 and 0.0984 μg cm-2. Limits of detection (LOD) were calculated to be 7.07 and 2.42 μg ml-1 and the limits of quantification (LOQ) were 21.43 and 7.33 μg ml-1 RPG, for CAA method and DDQ method, respectively. Validation results demonstrated that the inter day and intra day accuracy were up to 97.56%. The precision determined did not exceed 2.5% of RSD. The methods were successfully used for the determination of RPG in tablet form and the results were in good agreement with the label claims as shown by the recoveries which were in the range of 99.22- 102.8% with standard deviation values < 2%. The accuracy of the method was confirmed by recovery studies via standardaddition procedure with excellent recovery 98.24-104.0 ± 1.08-3.35. |
