Stability indicating reversed-phase liquid chromatographic determination of metronidazole benzoate and diloxanide furoate as bulk drug and in suspension dosage form

J Pharm Biomed Anal. 2005 Sep 15;39(3-4):819-23. doi: 10.1016/j.jpba.2005.05.029.

Abstract

A selective, precise and accurate isocratic RP-HPLC method has been developed and validated for the simultaneous determination of metronidazole benzoate (MB), diloxanide furoate (DF), methyl paraben (MPn) and propyl paraben (PPn) in suspension. The cis/trans isomerization phenomenon for DF has also been presented. The method uses as stationary phase a Supelco LC-18 DB (15 cm x 4.6 mm) 5 microm column and as a mobile phase a buffer-acetonitrile mixture (70:30, v/v) adjusted to pH of 2.5 at a flow rate of 2.0 mLmin(-1). The buffer is a 0.005 M KH2PO4 solution. The four analytes were well resolved from the degraded solutions peaks. The excepients present in the formulation do not interfere with the assay procedure. The linearity range (n=3) is (0.20130-1.20779 mgmL(-1)) for MB with R of 0.99985; (0.15790-0.94740 mgmL(-1)) for DF with R of 0.99987; (0.01131-0.06788 mgmL(-1)) for MPn with R of 0.99987 and (0.00126-0.00756 mgmL(-1)) for PPn with R of 0.99991. Precision (n=6) was 0.87% for MB; 1.15% for DF; 1.32% for MPn and 1.27% for PPn. The percentage recoveries (n=3) were 99.1% for MB; 99.6% for DF; 99.1% for MPn and 98.7% for PPn. The proposed method can be utilized for the routine analysis of the four analytes in pharmaceutical dosage form.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Benzoates / chemistry
  • Buffers
  • Calibration
  • Chemistry, Pharmaceutical / methods*
  • Chromatography
  • Chromatography, High Pressure Liquid / methods*
  • Dosage Forms*
  • Drug Stability*
  • Furans / analysis*
  • Furans / chemistry
  • Hydrogen-Ion Concentration
  • Metronidazole / analysis*
  • Metronidazole / chemistry
  • Models, Chemical
  • Parabens / analysis
  • Pharmaceutical Preparations / analysis*
  • Placebos
  • Reproducibility of Results
  • Solvents
  • Stereoisomerism
  • Time Factors

Substances

  • Benzoates
  • Buffers
  • Dosage Forms
  • Furans
  • Parabens
  • Pharmaceutical Preparations
  • Placebos
  • Solvents
  • Metronidazole
  • methylparaben
  • diloxanide furoate
  • propylparaben