Romanian Society of Pharmaceutical Sciences
 

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THE DEVELOPMENT AND VALIDATION OF A RAPID HPLC METHOD FOR DETERMINATION OF PIROXICAM

GEORGE TRAIAN ALEXANDRU BURCEA DRAGOMIROIU1, ADINA CIMPOIEŞU1*, OCTAV GINGHINĂ2, CORNELIU BALOESCU1, MARIA BÂRCĂ1, DANIELA ELENA POPA1, ANNEMARIE CIOBANU1, VALENTINA ANUŢA3

1.Department of Drug Control, Faculty of Pharmacy, “Carol Davila” University of Medicine and Pharmacy Bucharest, 6 Traian Vuia Street, 020956, Bucharest, Romania
2.Department of Oncological Surgery, Faculty of Dental Medicine, “Sf. Ioan” Hospital, “Carol Davila” University of Medicine and Pharmacy, 13 Vitan-Barzesti Street, 042122, Bucharest, Romania
3.Department of Physical Chemistry, Faculty of Pharmacy, “Carol Davila” University of Medicine and Pharmacy Bucharest, 6 Traian Vuia street, 020956, Bucharest, Romania

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The present paper presents the development and validation of a novel fast, sensitive and accurate HPLC-UV method for the quantitative determination of Piroxicam in bulk materials and pharmaceutical formulations. Development of the chromatographic method was based on a design of experiments (DOE) approach, using the Box-Behnken design in order to identify the significant parameters for the optimization, by simultaneously registering retention time, peak symmetry, and resolution of the chromatographic separation, number of theoretical plates and capacity factor of the first eluting peak as responses. Derringer's desirability function (d) was used in order to identify the areas in the design region where the process is likely to give the optimal results. The mobile phase consisting in a trifluoroacetic acid: acetonitrile mixture at a 60:40 (v/v) ratio, delivered isocratically at a flow rate of 1.1 mL/min, and a column temperature of 40°C were found to be the optimum experimental conditions for the separation. The method was fully validated in accordance with the current ICH guidelines in terms of specificity, linearity, precision, accuracy, limits of detection/quantitation, and system suitability. The Piroxicam stability studies revealed that the active substance is stable in methanol solutions, as well as in acidic environment (in both mobile phase and in 0.1M HCl solution). The tested temperature conditions (from 4 to 37°C) had no significant impact on Piroxicam stability. However, direct exposure to sunlight induced an approximately 25% degradation within 4 hours. The method was found suitable for stability studies and for routine quality control analysis for products of similar type and composition.