Abstract
Abstract A simple, highly robust (quality by design (QbD) approach), precise and accurate method using high performance liquid chromatography coupled to mass spectrometry has been established for the simultaneous separation, identification and quantitation of a Torsemide (TOR), spironolactone (SPI) and their degradant impurities. The chromatographic separations of drugs and impurities were achieved on a inertsil ODS-3 µm C18, 150 mm × 4.6 mm, while the isocratic elution using a ternary mobile phase mixture of methanol, acetonitrile and water (5:3:2 v/v/v) at a flow rate of 0.2 mL/min was adopted for achieving optimum separations. The quantitation of torsemide and spironolactone was accomplished by UV detection at 254 nm and identification of the degradants were done by comparing identical mass in mass spectrometer. The recoveries of the torsemide and spironolactone were obtained higher than 98 % with good validation parameters; linearity (r2>0.994), LOD and LOQ was 10 and 33 ng for TOR and 75 and 248 ng for SPI respectively. The quality by design (QbD) approach has been successfully utilized to prove the method is robust even deliberate changes in critical parameters.
Highlights
Materials and methodsTorsemide (TOR) and Spironolactone (SPI) (Figure 1) are Instruments most widely used drug for treatment of diurectics [1].HPLC chromatographA GL Science (USA) HPLC chromatograph was used for the separations in this study
A simple, highly robust (quality by design (QbD) approach), precise and accurate method using high performance liquid chromatography coupled to mass spectrometry has been established for the simultaneous separation, identification and quantitation of a Torsemide (TOR), spironolactone (SPI) and their degradant impurities
The quantitation of torsemide and spironolactone was accomplished by UV detection at 254 nm and identification of the degradants were done by comparing identical mass in mass spectrometer
Summary
A GL Science (USA) HPLC chromatograph was used for the separations in this study. It was equipped with binary pump, which were capable to adjust the flow rate (0.01 to 5 mL/min.). It is equipped with an Autosampler with a capacity of accurately injecting the. U. Bihola et al.: HPLC – Quality by Design Approach sample volume of 50 nL to 100 μL into the analytical column. The analytes were detected by using fibre optics based UV detector. The effluent coming from the HPLC was injected in the MS/MS for detection of any impurity if present
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