Development and validation of spectrophotometric and high-performance column liquid chromatographic methods for the simultaneous determination of dienogest and estradiol valerate in pharmaceutical preparations


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ÇAĞLAYAN M. G. , Paibivik I. M. , ONUR F.

Journal of AOAC International, vol.93, no.3, pp.862-868, 2010 (SCI-Expanded) identifier identifier

  • Publication Type: Article / Article
  • Volume: 93 Issue: 3
  • Publication Date: 2010
  • Doi Number: 10.1093/jaoac/93.3.862
  • Journal Name: Journal of AOAC International
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Page Numbers: pp.862-868
  • Lokman Hekim University Affiliated: Yes

Abstract

Simultaneous determination of dienogest (DIE) and estradiol valerate (EST) in sugar-coated tablets was performed by using HPLC and spectrophotometry. In HPLC, the separation was achieved on an ACE C8 column using the mobile phase acetonitrile-NH4NO3 (0.03 M, pH 5.4; 70 + 30, v/v) at a flow rate of 2 mL/min. The detection wavelength was 280 nm, and cyproterone acetate was selected as an internal standard. The linearity range was 3.0-45.0 μg/mL for DIE and 18.0-100.0 μg/mL for EST. As spectrophotometric methods, two chemometric methods, principal component regression and partial least-squares, were developed. In the chemometric techniques, the concentration data matrix was prepared by using mixtures containing these drugs in methanol-water (3 + 1, v/v). The absorbance data matrix corresponding to the concentration data matrix in these methods was obtained by the measurement of absorbances in their zero-order spectra; then, the calibration was obtained by using the data matrix for the prediction of unknown concentrations of DIE and EST in their binary mixture. Working ranges were found as 2.0-24.0 μg/mL for DIE and 20.0-270.0 μg/mL EST in the methods. These three developed methods were validated and successfully applied to a pharmaceutical preparation, a sugar-coated tablet, and the results were compared with each other.