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Development and validation of an isocratic HPLC method for simultaneous determination of quaternary mixtures of antihypertensive drugs in pharmaceutical formulations

Anderson J. F. F., Gerlin M. C. G., Sversut R. A., Oliveira L. C. S., Singh A. K., Amaral M. S., Kassab N. M.

Acta Chromatographica

2017

Vol. 29, no. 1

95--110

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® C-18 column (100 mm × 4.6 mm, 2.6 μm). The mobile phase was composed of metanol-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 μg Ml-1 for atenolol (r = 0.9995), 0.30–12.00 μg Ml-1 for furosemide (r = 0.9997), 0.45–12.00 μg Ml-1 for losartan (r = 0.9995), and 0.45–12.0 μg 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.

Perspektywy wytwarzania biogazu przy uwzględnieniu mechanizmów reakcji w zakresie analizy ilościowej i jakościowej procesów fermentacji

Pilarski K., Adamski M.

Journal of Research and Applications in Agricultural Engineering

2009

Vol. 54, nr 2

81-86

W pracy przedstawiono wyniki badań laboratoryjnych wpływu składu chemicznego mieszanin substratów na procesy fermentacji. Badania przeprowadzono w zakresie obniżonej do około 6% zawartości suchej masy. Porównanie przebiegu fermentacji zakiszanej kukurydzy oraz odpadów celulozowych wykazały, iż istotny wpływ na wydajność fermentacji ma skład mieszaniny substratów. Przy porównaniu wskazano na inhibujące działanie pulpy celulozowej.

The results of laboratory investigations of influence of chemical constitution of substrates mixture on processes of fermentation. Investigations showed that essential influence on efficiency of fermentation has the composition of substrates mixture.