DEVELOPMENT AND VALIDATION OF KETOROLAC TROMETHAMINE ANALYSIS METHODS USING HPLC AND TEST ITS STABILITY

Abstract

Determination of ketorolac tromethamine levels based on United States Pharmacopeia (USP) using L7 column 4.6 mm x 25 cm; 5 μm with mobile phase tetrahydrofuran and buffer (30:70). Tetrahydrofuran has oxidative properties and has a high UV limit and the presence of peroxide impurities in it can affect the stability of the analyte so that the use of tetrahydrofuran is often avoided. Therefore, a method for analyzing ketorolac tromethamine was developed by applying of High Performance Liquid Chromatography (HPLC) using C18 column with acetate buffer pH 4.2 and methanol (20:80) as mobile phase, flow rate 1.0 mL/minute, wavelength 318 nm, and 10 μL injection volume. The validation results obtained a linearity value (r) 0.9982, value of LOD is 9.61 μg/mL and LOQ is 29.11 μg/mL. The results of precision test obtained %RSD equal to 0.776% and the accuracy test of the sample concentrations 80%, 100% and 120% show the %recovery are 94,79%, 99,42% and 92,83%, respectively. New degradants were formed with acid exposure of 80.66%, base exposure of 59.30%, temperature exposure (70-90°C for 3 hours) are 1.28%, 15.06%, and 18.40 %, respectively. Oxidation exposure (H₂O₂ 1%, 3% and 5%) are 11.36%, 13.98% and 14.79%, respectively. All the research results can be concluded that the method development and validation results can be used for the analysis of ketorolac tromethamine and testing its stability.