Quantitative determination of some pharmaceutical piperazine derivatives through complexation with iron(III) chloride.

A simple, accurate and sensitive spectrophotometric method has been developed for the determination of three pharmaceutical piperazine derivatives, namely ketoconazole (KC), trimetazidine hydrochloride (TMH) and piribedil (PD). This method is based on the formation of yellow orange complexes between iron(III) chloride and the investigated drugs. The optimum reaction conditions, spectral characteristics, conditional stability constants and composition of the water soluble complexes have been established. The method permits the determination of KC, TMH and PD over a concentration range 1-15, 1-12 and 1-12 microg ml(-1), respectively. Sandell sensitivity is found to be 0.016, 0.013 and 0.013 microg cm(-2) for KC, TMH and PD, respectively. The method was sensitive, simple, reproducible and accurate within +/-1.5%. The method is applicable to the assay of the three drugs under investigation in different dosage forms and the results are in good agreement with those obtained by the official methods (USP and JP).

Poly(vinyl chloride) ion-selective electrodes for piribedil determination.

Piribedil (PD) ion-selective electrodes have been constructed from poly(vinyl chloride) matrix membrane containing piribedil-tetraphenylborate (PD-TPB) as the electroactive component with dibutylphthalate or dioctylphthalate as the plasticizing solvent mediator. The electrodes displayed a linear response over the concentration range 2.0 x 10(-5) to 10(-2) M PD. The working pH ranges of the electrodes were 3.5-6.4 and 3.0-6.0, and the isothermal coefficients of the cells were 0.00129 and 0.00096 V/degrees C respectively. The electrodes were used for the determination of the diprotonated PD species, the most successful being that based on dioctylphthalate solvent mediator. The electrodes show a linear response over the concentration range of 8.0 x 10(-6) to 10(-2) M PD, with Nernstain slope 30 mV/PD concentration decade when preconditioned by soaking in distilled water for 30 min. The electrodes exhibit good selectivity for the PD with respect to a large number of inorganic cations and organic substances of biological fluids. Piribedil is determined successfully in pure solutions and in tablets or in biological fluids using the standard additions and potentiometric titration methods. The membrane withstood soaking in distilled water for more than 5 months.

Ion-pair formation of Bi(III)-iodide with some nitrogenous drugs and its application to pharmaceutical preparations.

A systematic spectrophotometric study on the ion-pair formation of Bi(III)-iodide with amineptine hydrochloride, piribedil and trimebutine maleate is carried out. The optimal experimental conditions pH, concentration of Bi(III) nitrate, potassium iodide; and the nature and amount of organic solvent have been studied. The ion pairs are soluble in 1,2-dichloroethane and the optimum pH range is 2.0-2.8. By application of the methods of Sommer and Job involving non-equimolar solutions, the conditional stability constant (log K') of the Bi(III) piridedil ion pair (1:1) at the optimum pH of 2.4 and an ionic strength (mu) 0.1 M, was found to be 5.436. The validity of Beer's law has been tested in the concentration range 5-50 microg ml(-1) in the organic layer, the relative standard deviation is less than 1%. The method is applied to the determination of these drugs in tablets without interference.

Spectrophotometric determination of some pharmaceutical piperazine derivatives through charge-transfer and ion-pair complexation reactions.

Simple and sensitive spectrophotometric methods are described for the assay of three piperazine derivatives; ketoconazole, piribedil and prazosin hydrochloride based on charge-transfer and ion-pair complexation reactions. The first method is based on the reaction of the basic drug with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) in acetonitrile. The orange-red colour formed due to the formation of charge-transfer complex showed maximum absorbance at 460 nm. The second method is based upon the interaction of the basic drug in dry chloroform with bromophenol blue (BPB) in the same solvent to produce a stable yellow ion-pair complex which absorbs at 410 nm. Beer's law was obeyed for both methods and the relative standard deviations were found to be less than 1%. The two methods can be applied to the analysis of tablets, with no evidence of interference from excipients. A more detailed investigation of the complex was made with respect to its composition, association constant and free energy change.