Stability Indicating RP-HPLC Method for Quantitative Estimation of Lenalidomide and Its Impurities in Solid Dosage Form
Pharmaceutical Science-Analytical chemistry
DOI:
https://doi.org/10.22376/ijlpr.2023.13.4.P29-P42Keywords:
Lenalidomide, determination of related substances, Forced degradation, LOD and LOQ, liquid chromatography.Abstract
The main aim and objectives of the research are to develop an effective, sensitive, economical, and simple reverse-phase HPLC method developed for determining and quantifying Lenalidomide impurities in Lenalidomide solid dosage formulations. The lack of research work and no compendial methods available for estimating this drug influenced the current research investigation to give a simple, sensitive, rapid, precise, accurate and robust gradient high-performance liquid chromatographic method for the determination and quantification of Lenalidomide and its impurities. Samples are analyzed using reverse phase (RP-HPLC) using stationary phase an Inertsil ODS-3V (150 x 4.6 mm, 3μm), and the mobile phase consists of two channels A and B. channel-A: pH 3.0 phosphate buffer and Channel-B: Acetonitrile: water (90:10 v/v) in the proportion of gradient elution. The flow rate is 1.0 mL/min. The column temperature was maintained at 40°C, and the sample cooler temperature was maintained at 5°C, injection volume of 20 μL, and wavelength of 210 nm. The developed HPLC method was validated concerning specificity, and the chromatograms were recorded for blank, placebo, standard, sample, and spiked sample solutions of Lenalidomide and its related substances. Specificity studies reveal that the peaks are well separated from each other. For precision, the results were found to be within acceptable limits. The limit of detection (LOD) and limit of quantitation (LOQ) for impurity-A 0.1124 μg/mL and 0.0371μg/mL, Impurity-B 0.2247μg/mL and 0.0742μg/mL, respectively. The linearity results for Lenalidomide and all the impurities in the specified concentration range are satisfactory, with a correlation coefficient greater than 0.99. The accuracy studies were shown as % recovery for Lenalidomide and its impurities at the specification level; the results obtained were within limits. Solution stability parameter was established; standard, sample, and spiked sample solutions are stable up to 48 hrs on a bench top at the refrigerator. Filter validation parameters were established, and the filtered spiked sample solutions are compatible with both 0.45 μm PVDF & 0.45 μm Nylon filters.
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