Development and validation of an LC-MS/MS method for the determination of adapalene in pharmaceutical forms for skin application

The development and validation of a liquid chromatography– tandem mass spectrometry (LC–MS/MS) method for the determination of adapalene in pharmaceutical forms for skin application were presented in this study. The MS/MS analysis of adapalene was performed by use of three mobile phases, consisted o...

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Bibliographic Details
Published in:Journal of the Serbian Chemical Society 2016-01, Vol.81 (10), p.1171-1181
Main Authors: Dobričić, Vladimir, Pajić, Nataša Bubić, Marković, Bojan, Vladimirov, Sote, Savić, Snežana, Vuleta, Gordana
Format: Article
Language:English
Subjects:
Acetonitrile
adapalene
Ammonium acetate
Flow velocity
Formic acid
Ions
LC-MS/MS determination
Linearity
Liquid chromatography
Mass spectrometry
MS/MS analysis
pharmaceutical forms for skin application
Pharmaceuticals
Phase composition
Reproducibility
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Summary:The development and validation of a liquid chromatography– tandem mass spectrometry (LC–MS/MS) method for the determination of adapalene in pharmaceutical forms for skin application were presented in this study. The MS/MS analysis of adapalene was performed by use of three mobile phases, consisted of acetonitrile and a) 0.1 % formic acid, b) 0.1 % trifluoroacetic acid and c) 20 mM ammonium acetate. The strongest signals of parent ion and dominant product ion were obtained in negative mode by use of the mobile phase c). The validation of this method was performed according to the ICH gu­idelines. Small variations of selected chromatographic parameters (concen­tra­tion of ammonium acetate, mobile phase composition, column temperature and flow rate) did not affect sig­nificantly the qualitative and quantitative sys­tem responses, which proved the method’s robustness. The method is specific for the determination of adapalene. The linearity was proved in the concentra­tion range of 6.7–700.0 ng mL-1 (r = 0.9990), with limits of detection and quantific­ation of 2.0 and 6.7 ng mL-1, respectively. The accuracy was con­firmed by cal­culated recoveries (98.4–101.5 %). The precision was tested at three levels: injection repeatability, analysis repeatability and intermediate pre­cision. The calcu­lated relative standard deviations were less than 1, 2 and 3 %, respect­ively.
ISSN:0352-5139
1820-7421
DOI:10.2298/JSC160215066D