Title : Comprehensive analytical and bioanalytical method validation for the quantification of linagliptin and empagliflozin in fixed-dose combinations
Abstract:
A comprehensive bioanalytical method was developed and validated for the simultaneous estimation of Linagliptin and Empagliflozin in fixed-dose combination formulations using UV spectrophotometry. This study emphasizes three distinct analytical approaches—Simultaneous Equation Method, Q-Absorbance Ratio Method, and Absorptivity Correction Method—to ensure accurate, precise, and reproducible quantification of both Active Pharmaceutical Ingredients (APIs) in a combined dosage form. The selected methods utilized a solvent system of methanol and distilled water (1:1 v/v) and an optimized wavelength range of 250–300 nm. In the Simultaneous Equation Method, the absorbance was measured at 297.4 nm and 277.2 nm, the respective λ-max of Linagliptin and empagliflozin. The Q-Absorbance Ratio Method was based on absorbance measurements, The isosbestic point is 2 at 287.4nm. The Absorptivity Correction Method involved compensating for overlapping spectra using known absorptivity’s to resolve individual drug concentrations. All three methods were validated as per ICH and USFDA guidelines. The calibration curves showed excellent linearity within the concentrations for both drugs. Recovery studies confirmed the methods’ accuracy, with percentage recovery values within the acceptable range of 98–102%. The precision was demonstrated by %RSD values below 2% for both intra-day and inter-day studies. The developed Empagliflozin in bulk and pharmaceutical dosage forms. Among them, the Q-Absorbance and Absorptivity Correction methods provide a rapid, economical, and non-destructive analytical tool suitable for routine quality control of Linagliptin and methods offer additional advantages in terms of simplicity and applicability in overlapping spectral conditions.
