QUALITY BY DESIGN BASED HPLC ASSAY METHOD DEVELOPMENT AND VALIDATION OF LINAGLIPTIN IN TABLET DOSAGE FORM

Sneha R. Barapatre, Anvesha V. Ganorkar and Krishna R. Gupta*

ABSTRACT

The current work describes QbD based simple and precise reversed-phase HPLC method development for routine analysis of Linagliptin in bulk drug and pharmaceutical formulations. Chromatographic separation was achieved on a ACE C18 column using isocratic elution with mobile phase containing mixture of phosphate buffer pH 7.2 adjusted with OPA 1% solution and methanol in the ratio (70:30v/v), with flow rate 1.0 mL/min and UV detection at 292 nm. The optimization of chromatographic method was carried by Box-Behnken design. The experimental design for the Assay method development utilizes three factors such as Mobile Phase (X1), Flow Rate (X2), and pH (X3) while Assymetry (Y1), Theoretical Plates (Y2), and Retention time (Y3) were used as responses. The developed experimental design was statistically analysed using ANOVA, counter plots and response surface plots. The method was optimized through system suitability test, linearity and assay of Linagliptin. The method was validated as per ICH guidelines for Accuracy, Precision, Ruggedness, LOD and LOQ which showed that proposed method was simple, sensitive, and highly robust for routine analysis of the Linagliptin.

Keywords: Linagliptin, Box-Behnken design, ANOVA, HPLC.