Simple and sensitive spectrophotometric method is described based on the coupling reaction of tetracycline hydrochloride(TC. HCl) with diazotized 4-aminopyridine in bulk and pharmaceutical forms. Colored azo dye formed during this reaction is measured at 433 nm as a function of time. Factors affecting the reaction yield were studied and the conditions were optimized. The kinetic study involves initial rate and fixed time (10 minutes) procedures for constructing the calibration graphs to determine the concentration of (TC. HCl). The graphs were linear for both methods in concentration range of 10.0 to 100.0 µg.mL-1. The recommended procedure was applied successfully in the determination of (TC. HCl) in itscommercial formulations.
A simple, fast and sensitive spectrophotometric method has been applied for the determination of tetracycline hydrochloride in its pure form and in pharmaceutical preparations. The method based on coupling reaction of the antibiotic with diazotized anthranilic acid to form a stable yellow azo dye which shows a maximum absorption at 419 nm. Uni- and multivariate approaches were followed in optimizing the experimental conditions. Under optimum experimental conditions obtained via multivariate (Central Composite Design), the linearity of the constructed calibration curve was in the range of 0.560 μg.mL-1 with molar absorptivity of 14619 L.mol-1.cm-1 and the value of detection limit was 0.2813μg.mL-1. The capability of the method for the analysis of real tetracycline samples was evaluated. The results show that the method could successfully be applied with no significant interference from the common excipients.
A reliable differential pulse polarographic (DPP) method has been developed and applied for the determination of ibuprofen IBU in dosage form with dropping mercury electrode (DME) versus Ag/AgCl. The best peak was found at cathodic peak of -1.18 V in phosphate buffer at pH=4 and 0.025M of KNO3 as supporting electrolyte. In order to obtaine the highest sensitivity, instrumental and experimental parameters were examined including the type and concentration of supporting electrolyte, pH of buffer solution, pulse amplitude and voltage step time. Diffusion current showed a direct linear relationship to ibuprofen concentration in the range of (5 – 30) μg. mL-1 (2.43× 10-5 – 1.45 × 10-4 mol·L–1) with correlation coefficient r= 0.9999, detection limit (S/N = 3) =3.40 μg. mL-1 (1.65 × 10-5 mol·L–1) and the value of precision in terms of relative standard deviation RSD%, ranged between 0.374-0.5176 %. The established DPP method offers an excellent analytical figure of merits as well as its successful applicability to examine two commercial drug forms (tablet and suspension) for the determination of ibuprofen.
Two simple methods for the determination of eugenol were developed. The first depends on the oxidative coupling of eugenol with p-amino-N,N-dimethylaniline (PADA) in the presence of K3[Fe(CN)6]. A linear regression calibration plot for eugenol was constructed at 600 nm, within a concentration range of 0.25-2.50 μg.mL–1 and a correlation coefficient (r) value of 0.9988. The limits of detection (LOD) and quantitation (LOQ) were 0.086 and 0.284 μg.mL–1, respectively. The second method is based on the dispersive liquid-liquid microextraction of the derivatized oxidative coupling product of eugenol with PADA. Under the optimized extraction procedure, the extracted colored product was determined spectrophotometrically at 618 nm. A linear plot within a concentration range of 0.05–1.65 μg.mL–1 (r = 0.9997) was constructed. The LOD and LOQ were 0.053 and 0.177 μg.mL–1, respectively. Both methods were tested for the analysis of eugenol in commercial personal-care products, and the results confirmed that the procedures are accurate, precise, and reproducible (RSD < 1%).
Two new simultaneous spectrophotometric methods for determination of Olanzapine and Ephedrine depend on third (D3) and fourth (D4) derivative of zero spectrum of two drugs were developed. The peak – to- base line, peak to peak and area under peak were found proportional with concentration of the drugs up to (4-24 µg/ml-1) at known experimental wavelengths. The results showed that the method was precise and accurate through RSD% (0.5026-4.0273),( 0.2399 6.9888) and R.E %(-2.3889-0.8333) ,) -2.9444-0.2273) while the LOD (0.0057- 0.8510 μg.ml-1), ( 0.0953-0.9844 μg.ml-1) and LOQ (0.0173- 2.5788μg.ml-1),( 0.5774-2.9829 μg.ml-1) were found for the two drugs respectively. The methods were applied ide to the determination of Olanzapine and Ephedrine in pharmaceutical preparations successfully.
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