Method Development and Acid Degradation Study of Doxofylline by RP-HPLC and LC-MS/MS

A simple, rapid and accurate RP-HPLC method was developed for the determination of doxofylline and acid degradation product. The method showed a linear response for concentrations in the range of 1-200 μg/ml using acetonitrile: formic Acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rate of 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis. The acid degradation product as well as pathway was characterized by LC-MS/MS.