RESUMEN
Two methods are presented for the determination of cefuroxime and cefadroxil in human urine using first (1D) derivative spectrophotometry and high-performance liquid chromatography. Cefuroxime and cefadroxil were determined by measurement of their first-derivative amplitude in 0.1 N sodium hydroxide at 292.5 and 267.3 nm, respectively in the concentration range of 2-10 microg ml(-1) for each drug. The HPLC method depends upon using a LiChrospher 100 RP-18 (5 microm) column at ambient temperature for cefuroxime and 35 degrees C for cefadroxil with mobile phases consisting of water-acetonitrile-acetic acid (85:15:0.1 v/v) at a flow rate of 1.5 ml min(-1) for cefuroxime; and 0.02 M potassium dihydrogen phosphate-acetonitrile (95:5 v/v) containing 0.003% (w/v) hexanesulphonic acid sodium salt and adjusted to apparent pH 3 with phosphoric acid at a flow rate of 2 ml min(-1) for cefadroxil. Quantitation was achieved with UV detection at 275 and 260 nm for cefuroxime and cefadroxil, respectively, based on peak area with linear calibration curves at the concentration ranges of 2-10 microg ml(-1) for cefuroxime and 5-20 microg ml(-1) for cefadroxil. The proposed methods were applied to the determination of dissolution rate for tablets and capsules containing each drug. The urinary excretion patterns as the cumulative amounts excreted have been calculated for each drug using the proposed methods.
Asunto(s)
Cefadroxilo/orina , Cefuroxima/orina , Cefalosporinas/orina , Cromatografía Líquida de Alta Presión/métodos , Espectrofotometría Ultravioleta/métodos , Adulto , Humanos , Masculino , Reproducibilidad de los Resultados , Sensibilidad y EspecificidadRESUMEN
Three methods are described for the simultaneous determination of mebeverine hydrochloride (MB) and sulpiride (SU) in combined pharmaceutical tablets. The first method depends on first-derivative ultraviolet spectrophotometry, with zero-crossing measurement method. The first derivative amplitudes at 214.2 and 221.6 nm were selected for the assay of MB and SU, respectively. Calibration graphs follow Beer's law in the range of 10-30 and 2-8 microg/ml(-1), and the linearity was satisfactory (r = 0.9999), for MB and SU, respectively. The second method was based on the application of the thin layer chromatographic separation of both drugs followed by the densitometric measurements of their spot areas. After separation on silica gel GF254 plates, using ethanol: diethyl ether: triethylamine (70:30:1 v/v) as the mobile phase, the chromatographic zones corresponding to the spots of MB and SU were scanned at 262 and 240 nm, respectively. The calibration function was established in the ranges of 4-12 microg for MB and 2-8 microg for SU. The third method was an internal standard procedure based on high performance liquid chromatographic separation of the two drugs on a reversed-phase, Bondapak CN column. The detection was done at 243 nm using buclizine hydrochloride as internal standard. All chromatographic methods showed good linearity, precision and reproducibility. No spectral or chromatographic interference from the tablet excipients were found. The proposed methods were successfully applied to the assay of commercial tablets and content uniformity test. The procedures were rapid, simple and suitable for quality control application.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Cromatografía en Capa Delgada/métodos , Fenetilaminas/análisis , Espectrofotometría Ultravioleta/métodos , Sulpirida/análisis , Anticonvulsivantes/análisis , Antipsicóticos/análisis , Control de Calidad , Comprimidos/análisisRESUMEN
Two methods are presented for the determination of cinchocaine HCl in presence of its acid-induced degradation product using first (1D) derivative spectrophotometry and high-performance liquid chromatography. Cinchocaine HCl was determined by measurement of its first derivative amplitude at the zero crossing point of 2-hydroxyquinoline-4-carboxylic acid diethylaminoethylamide as its acid degradation product (at 333.5 nm). The HPLC method depends upon using a mu Bondapak C18 column at ambient temperature with a mobile phase consisting of acetonitrile--0.01 M sodium acetate trihydrate (45:55, v/v) containing 0.06% (w/v) heptane sulphonic acid sodium salt and adjusted to apparent pH 4.5 with acetic acid at a flow rate 2 ml min-1. Quantitation was achieved with UV detection at 254 nm based on peak area. The HPLC method was applied for simultaneous determination of cinchocaine HCl, methylparaben and propylparaben. The two proposed methods were successfully applied to the determination of the cinchocaine HCl in laboratory-prepared mixtures in the presence of its acid degradation product and in cream. Moreover, the proposed methods were utilized to investigate the kinetics of the acid degradation process at different temperatures and the apparent pseudo first-order rate constant, half-life and activation energy calculated.
Asunto(s)
Anestésicos Locales/análisis , Técnicas de Química Analítica/métodos , Cromatografía Líquida de Alta Presión/métodos , Dibucaína/análisis , Espectrofotometría/métodos , Anestésicos Locales/química , Anestésicos Locales/farmacocinética , Dibucaína/química , Dibucaína/farmacocinética , Combinación de Medicamentos , Pomadas/química , Parabenos/análisis , Preparaciones Farmacéuticas/químicaRESUMEN
Derivative spectrophotometric, colorimetric and high performance liquid chromatographic methods, for the determination of the antihistaminic cetirizine dihydrochloride in tablet form were described. Spectrophotometrically, cetirizine was determined by the measurement of its first (1D) and second (2D) derivative amplitudes at 239 (peak) and 243-233 nm (peak-to-trough), respectively. The aqueous solutions obeyed Beer's law in the concentration ranges of 1.2-10.0 and 0.8-10.0 micrograms ml-1 for 1D and 2D measurements, respectively. The colorimetric procedure was based on measuring the absorbency of the coloured chromogen resulted from the reaction between cetirizine sodium salt in polar solvent (DMF) and chloranil at 556 nm. The relation with concentrations was linear over 120-250 micrograms ml-1. Optimization of the reaction conditions was studied. At the same time, investigation of the complex formed was made with respect to its composition and the associated constant. A simple liquid chromatographic assay has been developed for the determination of cetirizine dihydrochloride in the presence of one of its synthesis precursor (hydroxyzine hydrochloride). A Bondapak-C18 column was used with a mobile phase consisting of acetonitrile/0.01 M ammonium dihydrogen phosphate (32:68, v/v) containing 0.1% w/v tetrabutyl ammonium hydrogen sulphate adjusted to pH 3 with phosphoric acid at a flow rate of 2 ml min-1. With salicylic acid as internal standard, quantitation was achieved with UV detection at 230 nm based on the peak height ratios. Beer's law was obeyed in a concentration range of 3-35 micrograms ml-1 and the regression line equation was derived with a correlation coefficient of 0.9999. The validity of the methods was further confirmed using the standard addition method. The proposed procedures were successfully applied to the determination of cetirizine in bulk and tablet form, with high percentage of recovery, good accuracy and precision.