RESUMO
A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith Performance RP-18e [100 mm x 4.6 mm] column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water [44:56 v/v] at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of detection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 microL injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103%. The method offers a valuable alternative to the methodologies currently employed for separation and quantification of prednisolone and betamethasone in urine samples
RESUMO
This work studies the development of a simple and fairly rapid methodology for simultaneous determination/ separation of three frequently co-administered drugs; ciprofloxacin [CIP], paracetamol [PCT] and diclofenac sodium [DIG] using capillary electrophoresis [CE] with UV detection at 260 nm. Separation was achieved in only 6.5 min with a simple buffer of sodium tetraborate [50 mM] at pH 9.0. The Parameters affecting the separation and detection were optimized. The calibration curves were linear in the range of 5-500 microg/mL for CIP, 5-250 micro g/mL for PCT and 1-125 microg/mL for DIC sodium under the optimized conditions. The lower limit of detection [LOD] was found to be 1 microg/mL for CIP and PCT and 0.5 microg/mL for DIC. The method was successfully used for the analysis of drugs in commercial pharmaceutical formulations and simultaneously from patient's urine sample with RSD 0.5-2.4%. Results obtained with CE method are compared with standard HPLC procedure and were found in good agreement