ABSTRACT
A capillary zone electrophoresis (CZE) method was developed for the quantitative analysis of fosinopril sodium. Validation parameters of the CZE method were evaluated and compared to an existing LC method. In terms of precision and sensitivity. LC performance was superior to that of the CZE method for this application. The CZE method achieved better selectivity for several degradants of interest within a much shorter analysis time than did the LC method. Effects of detection wavelength, applied voltage and buffer concentration on optimization of the CZE method are presented. Effects of diluent composition on capillary loading and peak behaviour are also discussed.
Subject(s)
Fosinopril/analysis , Buffers , Chromatography, Liquid/methods , Electrophoresis/methods , Reproducibility of Results , Sensitivity and SpecificityABSTRACT
Surfactant-containing eluents are evaluated for possible application to direct serum injection using conventional reverse-phase columns. Serum albumin was quantitatively eluted at the column void volume by using surfactant concentrations below or above the critical micelle concentration, and organic solvents could be used in proportions as high as 40% (w/w). Surfactant choice, pH, and salt effects were also evaluated.
Subject(s)
Carbamazepine/blood , Chromatography, Liquid/methods , Serum Albumin/chemistry , Surface-Active Agents/chemistry , Xanthines/blood , Adsorption , Carbamazepine/analogs & derivatives , Hydrogen-Ion ConcentrationABSTRACT
Column switching is used in conjunction with surfactant containing mobile phases and traditional reverse phase LC columns to provide a highly reproducible and accurate analytical procedure for carbamazepine and its 10,11-epoxide in serum. This approach eliminates the tedious sample preparation steps commonly used in the analysis of drugs by HPLC, while providing a high degree of protein removal prior to the final analysis. Various pre-columns were investigated and a pellicular reverse phase column was found suitable for optimum concentration of drugs and removal of serum proteins. A variety of standard reverse phase columns could be used for the analytical separation. The separation of the drugs could be accomplished with a high degree of reproducibility. Tandem pre-column operation was demonstrated to give a sample throughput of 10 h-1.
Subject(s)
Carbamazepine/analogs & derivatives , Carbamazepine/blood , Drug Monitoring/methods , Chromatography, Liquid/instrumentation , Chromatography, Liquid/methods , Humans , Reproducibility of Results , Surface-Active Agents/analysisABSTRACT
Surfactant-containing eluents are evaluated for the analysis of carbamazepine in serum with conventional reversed-phase columns. Bovine serum was quantitatively eluted at the column void volume using surfactant concentrations in conventional reversed-phase eluents. The effect of pH, guard columns and column switching was evaluated with respect to separating and detecting clinical levels of the drug and its primary metabolite. Column lifetime was also investigated.
