Analytical Method Development and Validation of High-Performance Liquid Chromatography for SimultaneousDetermination of Ibuprofen and Baclofen

Abstract

Combining baclofen with ibuprofen offers synergistic pain relief by targeting both muscle spasms and inflammation, enhancing efficacy in managing musculoskeletal conditions. This study aims to develop and validate an analytical method for the separation and simultaneous determination of ibuprofen and baclofen in combination using high-performance liquid chromatography (HPLC) in pharmaceutical dosage forms. An HPLC analytical method was developed to simultaneously quantify ibuprofen and baclofen. The optimized method was validated in accordance with the International Conference on Harmonization (ICH) guidelines. The method was tested for validation parameters, including specificity, accuracy, precision, linear range, limit of detection, lower limit of quantification, and robustness. A simple HPLC method was developed to separate two active ingredients using a C18 stationary phase column (25 cm × 0.46 cm, 5 μm). The mobile phase consisted of methanol: buffer (pH 3 ± 0.05), and acetonitrile in a ratio of 5:30:65 (%v/v). The analysis was performed at 25 °C with a 1.5 mL/min flow rate. A 20 μL sample volume was injected and detected at 265 nm. The validation method was specific, precise, and accurate. The average recovery of the two ingredients was 100.5% [99.1-102.0]. The repeated tests of the two compounds at different concentrations showed a percentage relative standard deviation (%RSD) of less than 1%. The method demonstrated linearity for both ibuprofen and baclofen, with an R² value of 0.99. The linearity range was 12.5-150 μg/mL for baclofen, and was 100-1800 μg/mL for
ibuprofen. The lower limit of quantification (LLOQ) was 7 and 6 μg/mL for ibuprofen and baclofen, respectively. The limit of detection (LOD) was 2 μg/mL for both ingredients. The
developed method is simple, rapid, precise, and accurate. It can be used for routine analysis of a combination of ibuprofen and baclofen in pharmaceutical dosage forms.