Voltammetry and quantification of the contraceptive drug norethisterone in bulk form and pharmaceutical formulation

J Pharm Biomed Anal. 2007 Jan 17;43(2):499-505. doi: 10.1016/j.jpba.2006.07.049. Epub 2006 Sep 6.

Abstract

The electrochemical behavior of norethisterone at the mercury electrode was studied in the universal buffer of various pH values using dc-polarography, cyclic voltammetry and controlled-potential electrolysis. Norethisterone was reduced at the mercury electrode via the consumption of two electrons corresponding to reduction of the 3-keto-delta-4-group in the A-ring of the molecule. The pK(a) value (8.7) of norethisterone was determined from the polarographic and spectrophotometric measurements. A fully validated, simple, sensitive, precise and inexpensive square-wave adsorptive cathodic stripping (SWAdCS) voltammetry procedure was described for trace quantification of bulk norethisterone. The stripping voltammetry peak current of norethisterone in a universal buffer of pH 5 following its accumulation onto the hanging mercury drop electrode (HMDE) at -0.6 V (versus Ag/AgCl/KCl(s)) for 130 s showed a linear response with the concentration over the range 5 x 10(-9) to 3 x 10(-7)M norethisterone. Detection and quantitation limits of 1.5 x 10(-9) and 5 x 10(-9)M bulk norethisterone, respectively, were achieved. The proposed procedure was successfully applied for the assay of norethisterone in Steronate tablets without interference from excipients.

Publication types

  • Validation Study

MeSH terms

  • Buffers
  • Calibration
  • Chemistry, Pharmaceutical
  • Contraceptives, Oral, Synthetic / analysis*
  • Contraceptives, Oral, Synthetic / chemistry
  • Electrochemistry / instrumentation
  • Electrochemistry / methods*
  • Electrochemistry / standards
  • Electrodes
  • Hydrogen-Ion Concentration
  • Mercury
  • Models, Chemical
  • Molecular Structure
  • Norethindrone / analysis*
  • Norethindrone / chemistry
  • Pharmaceutical Preparations / chemistry
  • Polarography / methods
  • Reproducibility of Results
  • Tablets
  • Technology, Pharmaceutical / instrumentation
  • Technology, Pharmaceutical / methods*
  • Technology, Pharmaceutical / standards

Substances

  • Buffers
  • Contraceptives, Oral, Synthetic
  • Pharmaceutical Preparations
  • Tablets
  • Mercury
  • Norethindrone