SciELO - Scientific Electronic Library Online

 
vol.48 número1Validación de un método de análisis para la determinación de raloxifeno en una formulación cubanaTratamiento antimicrobiano en la meningoencefalitis, Hospital Militar Central "Dr. Luis Díaz Soto", 2004-2011 índice de autoresíndice de materiabúsqueda de artículos
Home Pagelista alfabética de revistas  

Servicios Personalizados

Revista

Articulo

Indicadores

  • No hay articulos citadosCitado por SciELO

Links relacionados

  • No hay articulos similaresSimilares en SciELO

Compartir


Revista Cubana de Farmacia

versión impresa ISSN 0034-7515

Resumen

CORREA CANO, Omar de Jesús; RUIZ CORREA, Adriana María  y  RESTREPO GARAY, Margarita María. Standardization of a HPLC method for quantitation of diclofenac in microdialysis samples through precolumn photoderivatization. Rev Cubana Farm [online]. 2014, vol.48, n.1, pp.23-33. ISSN 0034-7515.

Introduction: the diclofenac quantitation in small volume and low analyte concentration samples is complex and requires a simple, highly sensitive and reproducible analytical method. Objective: to standardize a high performance liquid chromatography with precolumn photoderivatization to quantitate diclofenac in small volume and low analyte concentration samples. Methods: diclofenac photoproducts were obtained by irradiating samples at l= 254 nm in quartz polytetrafluoroethylene (PTFE) and polyvinyl chloride (PVC) cells placed in different positions of the irradiation area for 6, 24 and 60 minutes respectively. For the separation of photoproducts, a C-18 Agilent Eclipse Plus column (5 µm, 150 mm; 4.6 µm id.) was used, with a mobile phase containing a mixture of acetonitrile and water pH 3.0 adjusted with ortho-phosphoric acid, in different proportions until the optimal one was found; the flow rate of mobile phase was 1.0 mL/min with column temperature of 30 °C. The sample injection volume was 20 µL. Photoproducts were detected through fluorescence with excitation and emission wavelength at 286 and 360 nm respectively. Results: diclofenac photodegradation in PTFE cells occurs within 6 minutes when solutions are irradiated at 254 nm in the central part of the irradiation area. The separation of the three major photoproducts was accomplished using a mobile phase of acetonitrile: water adjusted with ortho-phosphoric up to pH= 3.0;65:35. The photoproduct at 3.4 minutes was eluted at high stable concentrations, with a linear trend presented in an area graph versus diclofenac concentration in the range of 1.25-500 ng/mL. Conclusions: a new HPLC-method for quantitation of diclofenac in small volume and low concentration samples was standardized; it may undergo validation process.

Palabras clave : PTFE; diclofenac; fluorescence; HPLC; microdialysis.

        · resumen en Español     · texto en Español     · Español ( pdf )