Speciation of Sb(III) and Sb(V) in meglumine antimoniate pharmaceutical formulations by PSA using carbon nanotube electrode.

摘要

A new and simple electroanalytical method for speciation of Sb(III) and Sb(V) in pharmaceutical formulation by potentiometric stripping analysis (PSA) using a multiwall carbon nanotube paste electrode was developed. All instrumental and chemical parameters influencing the performance of the method were carefully assessed and optimized. Trivalent antimony was determined in acid medium (pH 3.6) under the optimized condition (deposition potential of -0.7 V, deposition time of 180 s, ionic strength of 0.3M and oxidant mercury concentration of 10 mg l(-1)). Total antimony was determined after quantitative reduction of Sb(V) with l-cysteine (1.5%, w/v) and its concentration was calculated from difference between the total antimony and Sb(III). The developed method provided two distinct linear calibration one ranging from 10 up to 50 microg l(-1) and other from 100 up to 800 microg l(-1) with respective correlation coefficient of 0.9978 and 0.9993, presenting a detection limit of 6.2 microg l(-1). Repeatability for the six independent samples expressed in terms of relative standard deviation was found to be 3.01 and 1.39% for 40.0 and 300.0 microg l(-1) antimony concentration, respectively. Results on the effect of foreign substances [Al(III), Mg(II), Fe(III), Cd(II), Zn(II) and meglumine] on analytical signal of antimony showed no interference even using high content of foreign ions in the analyte:interferent ratio up to 1:100. The proposed method was successfully applied for the speciation of Sb(III) and Sb(V) in pharmaceutical formulation and the accuracy was assessed from addition and recovery tests as well as comparing with graphite furnace atomic absorption spectrometry (GF AAS) technique used as reference analytical method.