Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
11027367 | Journal of Pharmaceutical and Biomedical Analysis | 2019 | 22 Pages |
Abstract
A capillary electrophoresis method was developed and validated for the determination of the purity of dapoxetine with regard to the related substances (3S)-3-amino-3-phenylpropan-1-ol, (3S)-3-(dimethylamino)-3-phenylpropan-1-ol, 1-naphthol and the enantiomer (R)-dapoxetine. The separation was based on a dual selector system, which was optimized by a fractional factorial resolution Vâ+âdesign followed by a central composite face centered design with star distance 1 and Monte Carlo simulations for defining the design space. The optimized background electrolyte consisted of a 50âmM sodium phosphate buffer, pH 6.3, containing 45âmg/mL sulfated γ-cyclodextrin and 40.2âmg/mL 2,6-dimethyl-β-cyclodextrin. Separations were carried out in a 23.5/32âcm, 50âμmâfused-silica capillary employing a separation voltage of 9âkV at 15â°C. Following robustness testing using a Plackett-Burman design the method was validated according to the International Council on Harmonization guideline Q2(R1) in the range of 0.05-1.0% relative to the dapoxetine concentration. The method was applied to the analysis of drug substance and a commercial tablet. Data regarding the enantiomeric purity of dapoxetine obtained by the capillary electrophoresis assay were comparable to the data obtained by an enantioselective HPLC method.
Related Topics
Physical Sciences and Engineering
Chemistry
Analytical Chemistry
Authors
Henrik Harnisch, Gerhard K.E. Scriba,