Fluorescence spectroscopy method for estimation of Ivabradine in bulk and the tablet dosage form.

A simple and sensitive spectrofluorimetric method has been developed for the estimation of Ivabradine HCl in bulk and the tablet dosage form. Ivabradine HCl in methanol produces fluorescence at 325 nm (λem) with excitation at 287 nm (λex). The linearity range was found to be 100-500 ng/ml with a correlation coefficient of 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) for the developed method were found to be 8.38 and 25.39 ng/ml, respectively. The developed method was found to be specific, sensitive, accurate, and precise. It was successfully used for the estimation of Ivabradine HCl in its tablet dosage form. The content of Ivabradine HCl in marketed formulations was found to be 101.25 ± 1.16 % of label claims.

Screening Design and Response Surface Methodology for the Simultaneous Estimation of Carvedilol and Ivabradine HCl by HPTLC Method.

The combination of carvedilol (CAR) and ivabradine (IVA) is used for a greater reduction in heart rate and for achieving better exercise capacity in a patient with chronic heart failure. Numerous reverse-phase high-pressure liquid chromatography (RP-HPLC) and hyphenated techniques have been reported for the simultaneous estimation of CAR and IVA, but the high-performance thin-layer chromatographic (HPTLC) method has not been reported yet. Hence, the robust HPTLC method has been developed by the implementation of an enhanced analytical quality by design approach based on the principles of analytical failure modes critical effect analysis (AFMCEA) and design of experiments (DoE) as per the upcoming ICH Q14 guideline. The AFMCEA was started by the identification of potential analytical failure modes followed by their critical effect analysis by a DoE-based screening design. The high-risk failure modes were optimized by DoE-based response surface methodology. The method operable design ranges and control strategy was framed for optimized chromatography conditions. The HPTLC method was validated as per ICH Q2 (R1) guideline. The HPTLC method was applied for the assay of FDC of CAR and IVA, and results were found in compliance with the labeled claim. The developed method can be used as an alternative to the published RP-HPLC method for quality control of FDC of CAR and IVA in the pharmaceutical industry.