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摘要
The objective of this study was to develop and validate an assay method for simultaneous determination of atenolol, furosemide, losartan, and spironolactone in pharmaceutical formulations. A reverse-phase high-performance liquid chromatography procedure was developed, using a Kinetex (R) C-18 column (100 mm x 4.6 mm, 2.6 mu m). The mobile phase was composed of methanol-water (75: 25 v/v, pH 3.0, adjusted with phosphoric acid), with a flow rate of 0.4 mL min(-1). All drugs were separated in less than 5 min. The method was validated according to International Conference on Harmonization (ICH) and Association of Official Analytical Chemists (AOAC) guidelines. The method showed linearity in a concentration range of 0.75-12.0 mu g mL(-1) for atenolol (r = 0.9995), 0.30-12.00 mu g mL(-1) for furosemide (r = 0.9997), 0.45-12.00 mu g mL(-1) for losartan (r = 0.9995), and 0.45-12.0 mu g mL(-1) for spironolactone (r = 0.9999). The method also showed repeatability and precision. The three-day average intra-day precisions were 101.35 +/- 0.74% for atenolol, 95.84 +/- 1.44% for furosemide, 98.90 +/- 1.16% for losartan, and 97.19 +/- 0.18% for spironolactone. Similarly, the inter-day precisions were 101.34 +/- 0.72% for atenolol, 95.84 +/- 0.1.50% for furosemide, 98.90 +/- 1.17% for losartan, and 97.19 +/- 0.83% for spironolactone. The method accuracy was also tested and validated -in this case, the average recovery values were 100.18 +/- 1.20% for atenolol, 99.83 +/- 1.54% for furosemide, 100.07 +/- 0.95% for losartan, and 99.94 +/- 0.93% for spironolactone. Finally, the method was successfully applied in the simultaneous determination of atenolol, furosemide, losartan, and spironolactone in magisterial formulas, as well as in commercial pharmaceutical formulations.
- 出版日期2017-3
