A simple, rapid and selective liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry （LC-APCI-MS） assay method has been developed and fully validated for the simultaneous quantification of ...A simple, rapid and selective liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry （LC-APCI-MS） assay method has been developed and fully validated for the simultaneous quantification of cefadroxil （CF） and clavulanic acid （CA） in human plasma. Analytes and internal standard （IS） were extracted from human plasma by solid- phase extraction （SPE） technique using Sam prep （3 mL, 100 mg） extraction cartridge. The extracted samples were chromatographed on a reverse phase Cls column using a mixture of methanol： acetonitrile： 2 mM ammonium acetate （pH 3.5） （25：25：50, v/v/v） as the mobile phase at a flow rate of 0.8 mL/min. Quantification of the analytes and IS were carried out using single quadrupole LC-APCI-MS through selected-ion monitoring （SIM） at m/z 362 and m/z 198, for CF and CA, respectively. Method validation was performed as per the FDA guidelines and the results met the acceptance criteria. Plasma concentration of CF and CA followed by the oral administration of CF/CA （500/125 mg） pill to healthy male volunteers （n= 12） was measured. Area under plasma concentration-time curve from 0 to 12 h （AUC0-12 h） and 0 h extrapolated to infinity （AUC0-∞） were calculated. The ratio of AUC0-12 h/AUC0-∞ was found to be 〉 85% for all the subjects, as recommended by the FDA guidelines.展开更多
A new simple and sensitive kinetic spectrophotometric method has been proposed for the determination of cefadroxil in pure form and pharmaceutical formulations. The proposed method is based on the formation of yellow ...A new simple and sensitive kinetic spectrophotometric method has been proposed for the determination of cefadroxil in pure form and pharmaceutical formulations. The proposed method is based on the formation of yellow coloured product (λmax = 410 nm) that resulted after addition of the reagent, which is composed of a mixture of Henna extract, sodium hydroxide and potassium permanganate, to cefadroxil aqueous solution. The experimental conditions have been optimized. Beer’s law is obeyed over the concentrations of 100 - 35 μg/ml, with a linear regression correlation coefficient of 0.996. The proposed method has been successfully applied for the determination of cefadroxil in pharmaceutical dosage forms.展开更多
文摘A simple, rapid and selective liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry （LC-APCI-MS） assay method has been developed and fully validated for the simultaneous quantification of cefadroxil （CF） and clavulanic acid （CA） in human plasma. Analytes and internal standard （IS） were extracted from human plasma by solid- phase extraction （SPE） technique using Sam prep （3 mL, 100 mg） extraction cartridge. The extracted samples were chromatographed on a reverse phase Cls column using a mixture of methanol： acetonitrile： 2 mM ammonium acetate （pH 3.5） （25：25：50, v/v/v） as the mobile phase at a flow rate of 0.8 mL/min. Quantification of the analytes and IS were carried out using single quadrupole LC-APCI-MS through selected-ion monitoring （SIM） at m/z 362 and m/z 198, for CF and CA, respectively. Method validation was performed as per the FDA guidelines and the results met the acceptance criteria. Plasma concentration of CF and CA followed by the oral administration of CF/CA （500/125 mg） pill to healthy male volunteers （n= 12） was measured. Area under plasma concentration-time curve from 0 to 12 h （AUC0-12 h） and 0 h extrapolated to infinity （AUC0-∞） were calculated. The ratio of AUC0-12 h/AUC0-∞ was found to be 〉 85% for all the subjects, as recommended by the FDA guidelines.
文摘A new simple and sensitive kinetic spectrophotometric method has been proposed for the determination of cefadroxil in pure form and pharmaceutical formulations. The proposed method is based on the formation of yellow coloured product (λmax = 410 nm) that resulted after addition of the reagent, which is composed of a mixture of Henna extract, sodium hydroxide and potassium permanganate, to cefadroxil aqueous solution. The experimental conditions have been optimized. Beer’s law is obeyed over the concentrations of 100 - 35 μg/ml, with a linear regression correlation coefficient of 0.996. The proposed method has been successfully applied for the determination of cefadroxil in pharmaceutical dosage forms.
