Analytical method development and validation for the estimation of Furosemide an anti-diuretic in Furosemide injection diluted with normal saline in presence of impurities by RP-HPLC

Resumo

This study was aimed to establish a simple, accurate, precise, robust and rapid reverse phase high performance liquid chromatographic method for the estimation of Furosemide in Furosemide injection diluted with normal saline and it was validated as per the parameters mentioned in the ICH guidelines such as system suitability, linearity, accuracy, precision, specificity, ruggedness and robustness and solution stability. The optimized chromatographic HPLC analysis was performed on Waters e2695 system equipped with Inertsil ODS-3V C18 column (250 cm x 150 mm; 5 µm particle size), with a mixture of 1% glacial acetic acid and acetonitrile in the ratio of 50%:50% v/v as the mobile phase, at the flow rate of 1.0 mL/min. The detection was performed at the wavelength of 272 nm and the retention time of Furosemide was found to be 7.03 min. The calibration plot gave linear relationship over the concentration range of 10-120 µg/mL with correlation coefficient of r² = 0.9998. The percentage purity of Furosemide in the given formulation was found to be 103.56 ± 0.6546. The amount of Furosemide in the given formulation for intraday and interday was found to be 102.45 ± 0.2291 and 102.67 ± 0.4041, respectively. The accuracy of the proposed method was determined by recovery studies and was found to be in the range of 100.14% to 101.01%. This indicates that there is no inteference was observed due to excipients used in formulation. The percentage of RSD was found to be less than 2 for all the parameters. All the impurities peak were separated well and no inteference were found with the retention time of Furosemide. The results of robustness, ruggedness and solution stability were found to be within the acceptance limit. Hence, the developed method was found to be simple, linear, accurate, precise, robust, rapid method for the analysis of Furosemide in Furosemide injection diluted with normal saline. In addition, the main feature of the developed method is lower run time with less solvent consumption.

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