Electrochemical oxidation of atorvastatin and its adsorptive stripping determination in pharmaceutical dosage forms and biological fluids

2011 ◽  
Vol 76 (12) ◽  
pp. 1633-1649 ◽  
Author(s):  
Dilek Eskiköy ◽  
Zehra Durmuş ◽  
Esma Kiliç

Electrochemical behavior of atorvastatin (AT) and optimum conditions to its quantitative determination were investigated using voltammetric methods. Some electrochemical parameters such as diffusion coefficient, surface coverage of adsorbed molecules, electron transfer coefficient, standard rate constant and number of electrons were calculated using the results of cyclic voltammetry. A tentative mechanism for the oxidation for AT has been suggested. The oxidation signal of AT molecule was used to develop fully validated, new, rapid, selective and simple square-wave anodic adsorptive stripping voltammetric (AdsSWV) and differential pulse anodic stripping voltammetric (AdsDPV) methods to direct determination of AT in pharmaceutical dosage forms and biological samples. For the AdsDPV and AdsSWV techniques, linear working ranges were found to be 1.0 × 10–7–5.0 × 10–6and 3.0 × 10–7–5.0 × 10–6mol l–1, respectively. The detection limits obtained from AdsDPV and AdsSWV were calculated to be 6.55 × 10–8and 1.53 × 10–7mol l–1, respectively. The methods were successfully applied to assay the drug in tablets, human blood serum and human urine.

2010 ◽  
Vol 75 (6) ◽  
pp. 685-702 ◽  
Author(s):  
Funda Öztürk ◽  
Ibrahim Hüdai Taşdemir ◽  
Zehra Durmuş ◽  
Esma Kiliç

Electrochemical behavior of disopyramide (DPA) and optimum conditions to its quantitative determination were investigated using voltammetric methods. Some electrochemical parameters such as diffusion coefficient, surface coverage of adsorbed molecules, electron transfer coefficient, standard rate constant and number of electrons were calculated using the results of cyclic and square-wave voltammetry. All studies were based on the quasi-reversible and adsorption-controlled electrochemical reduction signal of DPA at about –1.60 V vs Ag|AgCl at pH 10.0 in Britton–Robinson buffer. This adsorptive character of molecule was used to develop fully validated, new, rapid, selective and simple square-wave cathodic adsorptive stripping voltammetric (SWCAdSV) method to the direct determination of DPA in pharmaceutical dosage forms and biological samples without time-consuming steps prior to drug assay. Peak current of electrochemical reduction of DPA was found to change linearly with the concentration in the range from 7.15 × 10–8 mol l–1 (0.024 mg l–1) to 1.43 × 10–6 mol l–1 (0.49 mg l–1). Limit of detection (LOD) and limit of quantification (LOQ) were found to be 5.65 × 10–8 mol l–1 (0.019 mg l–1) and 1.88 × 10–7 mol l–1 (0.064 mg l–1), respectively. The method was successfully applied to assay the drug in tablets, human serum and human urine with good recoveries at about 100%.


Author(s):  
D. K. Sharma ◽  
Jasvir Singh ◽  
Pushap Raj

Objective: A new spectrophotometric method for the determination of propranolol hydrochloride (PRO) and metoprolol tartrate (MTP), beta blocker drugs, has been developed for their analysis in pharmaceutical dosage forms for the purpose of quality control and water samples for monitoring impact on environmental water quality of natural sources and in biological fluids for ascertaining their physiological performance.Methods: The method is based on the derivatization of the amino function present in these drugs to the corresponding yellow copper (I) drug dithiocarbamate derivative through reaction with carbon disulphide, pyridine and copper (I) perchlorate in aqueous acetonitrile and measuring absorbance at 406 nm for propranolol and 400 nm for metoprolol. The different experimental parameters affecting the development and stability of the colour were carefully studied and optimized.Results: The Beer’s law is obeyed in the range of 1.0-40.0 μg/ml of each drug solution with a correlation coefficient 0.999. The maximum relative standard deviations (RSDs) in the analysis of pure PRO and MTP were 1.01 and 1.52 % respectively. The recoveries of the drugs from pharmaceutical formulations, spiked water samples and biological fluids were in the range 98.0-100.5 % with RSDs in the range 0.23-1.94% indicating good accuracy and precision of the method.Conclusion: The instantaneous development of colour and its stability, well-established stoichiometry of the reaction and above simplicity and rapidity of procedures are some special attributes of the proposed method.


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