Validación de método cromatográfico por HPLC de la valoración e identificación del (1-(1β, 16α)-21-(acetiloxi)-11- hidroxi-2´-metil-5´H-pregna-1,4-dieno[17,16-d]oxazol-3,20- diona) en Deflazacort materia prima

Maya Alejandra Parga; Natalia  Afanasjeva

doi:10.22490/24629448.6920

Vol. 21 No. 40 (2023)

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2023-05-01

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Validation of the HPLC chromatographic method for the evaluation and identification of (1-(1β, 16α)-21-(acetyloxy)-11-hydroxy-2´-methyl-5´H-pregna- 1,4-dieno[17, 16-d]oxazole-3,20-diona) in Deflazacort raw material

DOI: https://doi.org/10.22490/24629448.6920

Section

Research Article (before OJS)

Maya Alejandra Parga Universidad del Valle

Natalia Afanasjeva Universidad del Valle

Introduction. Deflazacort (DFZ) is a synthetic ozaxolinic glucocorticoid derived from prednisolone, it has anti-inflammatory properties and acts as an immunosuppressant, is the raw material used as the active ingredient of products marketed in pharmaceutical forms such as tablets and oral suspensions. Objective. Validate the methodology analytical by high performance liquid chromatography (HPLC), for the identification and assessment of (1-(1β,16α)-21-(acetyloxy)-11-hydroxy-2´-methyl-5´H-pregna-1,4 -dieno[17,16-d] oxazol-3,20-diona) in Deflazacort raw material under tropical climate conditions. Methodology.
Using as mobile phase an isocratic mixture of methanol and water in a ratio of 80:20 with a flow of 1, 1mL/min, the column used was Luna® 5μm C8 100Ǻ 250 x 4.6mm, diode array detector at a wavelength of 245nm. Results. For linearity, a correlation coefficient
R ≥ 0.999 was obtained, the coefficient of variation did not exceed the RS D of 2.0% in the repeatability of the system and in intermediate precision between analysts, an RSD value <3.0% was identified, in accuracy a recovery percentage of 98.9% was found.
Conclusions. T he method is l inear, precise, exact, robust for a f low of 1.21mL/min a nd not for a flow of 0.99mL/min since it does not meet retention time. In the performance tests, Deflazacort showed low stability when exposed to degradation by basic hydrolysis with 1.0 N and 0.1 N NaOH solutions. The sample and the standard in solution showed to be stable at room temperature for two hours and refrigerated for three hours.

high pressure liquid chromatography, immunosuppressive drugs, statistics and numerical data, analytical methods

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Parga, M. A., & Afanasjeva, N. (2023). Validation of the HPLC chromatographic method for the evaluation and identification of (1-(1β, 16α)-21-(acetyloxy)-11-hydroxy-2´-methyl-5´H-pregna- 1,4-dieno[17, 16-d]oxazole-3,20-diona) in Deflazacort raw material. NOVA Biomedical Sciences Journal, 21(40), 119-139. https://doi.org/10.22490/24629448.6920

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Validation of the HPLC chromatographic method for the evaluation and identification of (1-(1β, 16α)-21-(acetyloxy)-11-hydroxy-2´-methyl-5´H-pregna- 1,4-dieno[17, 16-d]oxazole-3,20-diona) in Deflazacort raw material

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