Journal of the Brazilian Chemical Society (Jan 2006)

Studies of zinc(II) in pharmaceutical and biological samples by extractive spectrophotometry: using pyridoxal-4-phenyl-3-thiosemicarbazone as chelating reagent

  • Sarma L. Subramanyam,
  • Kumar J. Rajesh,
  • Reddy K. Janardhan,
  • Thriveni T.,
  • Reddy A. Varada

Journal volume & issue
Vol. 17, no. 3
pp. 463 – 472

Abstract

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Pyridoxal-4-phenyl-3-thiosemicarbazone (PPT) is proposed as a new sensitive reagent for the sensitive extractive spectrophotometric determination of zinc(II). PPT reacts with zinc(II) in the pH range 5.0-6.0 to form a yellow colored complex, which was well extracted into n-butanol. The absorbance value of Zn(II)-PPT complex was measured at different intervals of time at 430 nm, to ascertain the stability of the complex. It was observed that the color development was instantaneous and stable for more than 48 h. The system obeyed Beer's law up to 6.0 µg mL-1 of zinc(II), with an excellent linearity in terms of correlation coefficient value of 0.999. The molar absorptivity and Sandell's sensitivity of the extracted species is 1.6 X 10(4) L mol-1 cm-1 and 4.085 X 10-3 µg cm-2 at 430 nm. The detection limit of the method is 0.04 µg mL-1. To assess precision of the method, determinations were carried out at different concentrations; the relative standard deviation does not exceed 3.1%. The composition of the zinc(II) complex with PPT was studied by the method of Job's continuous variation, molar ratio method, Asmus' method and slope ratio method. It has been satisfactorily applied for the determination of zinc(II), when present alone or in presence of diverse ions, which are usually associated with zinc(II) in pharmaceutical and biological samples. Various certified reference materials (NIST 1573, NBS 1572 and NIST SRM 8435) have been tested for the determination of zinc for evaluating the accuracy of the developed method. The results of the proposed method are in agreement with flame atomic absorption spectometry.

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