Development and validation of a stability-indicating HPTLC assay method for idebenone

Abstract

A simple, selective, precise, and stability-indicating high-performance thin layer chromatographic (HPTLC) method has been established and validated for the analysis of idebenone in bulk drug and formulations. The compounds were analyzed on aluminum-backed silica gel 60 F 254 plates with petroleum ether-methanol (4:1, v/v) as mobile phase. Densitometric analysis of idebenone was performed at 282 nm. Regression analysis data for the calibration plots were indicative of good linear relationship between response and concentration over the range of 200-600 ng per spot. The correlation coefficient (r 2 ) was 0.989 ± 0.002. The values of slope and intercept of the calibration plots were 2.386 ± 0.0435 and 577.733 ± 19.545, respectively. The method was validated for precision, accuracy, robustness, and ruggedness. The limits of detection and quantification were 14.642 and 44.369 ng, respectively. Idebenone was subjected to acid, base, peroxide, and sunlight degradation. In stability tests, the drug was susceptible to acid and basic hydrolysis, oxidation, and photodegradation.

Analytical Method and Stability Study for Oral Suspension of Idebenone in Syrspend

“…Stability studies are essential to know the effect of storage conditions of a galenic product to determine the appropriate shelf life and storage conditions [14]. The International Conference on Harmonization (ICH) [15] suggests that analytical test procedures for stability samples should be fully validated [16]. There are reported methods for the determination of ubiquinones by HPLC-UV-vis [4,17,18], colorimetric methods [19], HPTLC [16], and, finally, GC-MS or LC-MS [3,16,20].…”

“…The International Conference on Harmonization (ICH) [15] suggests that analytical test procedures for stability samples should be fully validated [16]. There are reported methods for the determination of ubiquinones by HPLC-UV-vis [4,17,18], colorimetric methods [19], HPTLC [16], and, finally, GC-MS or LC-MS [3,16,20]. LC-MS appears to be the gold standard for sta-bility studies of pharmaceutical preparations thanks to the ability to quantify analytes in solution, and to the high sensitivity and reproducibility inherent of MS. A fully validated HPLC-MS/MS method has been applied but for pharmacokinetic study [3] in plasma and urine samples to detect IDB and metabolites as reported above.…”