Development and validation of spectrophotometric and high-performance column liquid chromatographic methods for the simultaneous determination of dienogest and estradiol valerate in pharmaceutical preparations.
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 microg/mL for DIE and 18.0-100.0 microg/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 microg/mL for DIE and 20.0-270.0 microg/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.
Cağlayan
Mehmet Gökhan
MG
University of Ankara, Faculty of Pharmacy, Department of Analytical Chemistry, Tandogan, Ankara, Turkey.
Palabiyik
Ismail Murat
IM
Onur
Feyyaz
F
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004958:Estradiol / Q000031:analogs & derivatives* / Q000032:analysis; D016018:Least-Squares Analysis; D009277:Nandrolone / Q000031:analogs & derivatives* / Q000032:analysis; D004364:Pharmaceutical Preparations / Q000032:analysis; D025341:Principal Component Analysis; D013053:Spectrophotometry / Q000379:methods*
D004364:Pharmaceutical Preparations; C023635:dienogest; D004958:Estradiol; D009277:Nandrolone