Stability-indicating method for the analysis of amorolfine and its N-oxide degradation product

Rafaela Zimmermann; Fernanda Battisti; Pamela Lukasewicz; Saulo F. Andrade; Diogo Miron; Elfrides Eva Scherman Schapoval

doi:10.22456/2527-2616.128737

Authors

Rafaela Zimmermann Graduate Program in Pharmaceutical Sciences, Pharmaceutical Quality Control Laboratory, School of Pharmacy - Universidade Federal do Rio Grande do Sul
Fernanda Battisti Graduate Program in Pharmaceutical Sciences - Universidade Federal do Rio Grande do Sul
Pamela Lukasewicz Graduate Program in Pharmaceutical Sciences - Universidade Federal do Rio Grande do Sul
Saulo F. Andrade Graduate Program in Pharmaceutical Sciences - Universidade Federal do Rio Grande do Sul
Diogo Miron Graduate Program in Pharmaceutical Sciences - Universidade Federal do Rio Grande do Sul
Elfrides Eva Scherman Schapoval Graduate Program in Pharmaceutical Sciences, Pharmaceutical Quality Control Laboratory, School of Pharmacy - Universidade Federal do Rio Grande do Sul

DOI:

https://doi.org/10.22456/2527-2616.128737

Keywords:

Amorolfine, N-oxide, HPLC, mass spectrometry, Loceryl

Abstract

This work aimed to validate an ionic pairing stability-indicating method for determining amorolfine (AMF) in topical formulations by HPLC-DAD. The tailing factor, capacity factor, and theoretical plates were optimized by employing the desirability function. AMF was quantified in a hydrophilic formulation produced in our laboratory and Loceryl® cream and lacquer. Reverse-phase HPLC method with detection at 218 nm showed selectivity (peak purity> 995), robustness (RSD <2.0%), linearity (35–325 μg.mL-1 ), accuracy (≈100.0%), precision (RSD <2.0%) and limit of quantitation of 750 ng.mL-1 . Forced degradation of AMF in hydrogen peroxide resulted in a degradation product with pH-dependent kinetics. The N-oxide degradation product was purified and identified by mass spectrometry (MS) and hydrogen and carbon nuclear magnetic resonance (1H and 13C NMR).

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