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J Chromatogr A ; 1649: 462227, 2021 Jul 19.
Artigo em Inglês | MEDLINE | ID: mdl-34038780

RESUMO

A robust and confirmative method was established for the determination of six acetylgestagen residues, namely, flurogestone acetate (FGA), megestrol (MA), melengestrol acetate (MGA), chlormadinone acetate (CMA), medroxyprogesterone (MPA), and hydroxyprogesterone acetate (HPA) in animal-derived matrix samples by utilizing enhanced matrix removal lipid (EMR-lipid) clean-up in combination with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The analytes were extracted with acetonitrile, purified with a EMR-lipid cartridge, and separated with a reversed-phase C18 column. The limit of quantification (S/N ≥ 10) for CMA, FGA, HPA, MA, and MGA in all matrices was 0.5 ng/g, and for MPA, it was 1.0 ng/g; the limit of detection (S/N ≥ 3) for CMA, FGA, HPA, MA, and MGA in all matrices was 0.1 ng/g, and for MPA, it was 0.2 ng/g. The recoveries were between 61.0% and 114.8%, and the relative standard deviations (RSDs) were below 12%. The method was calibrated in a matrix-assisted standard solution in various linear ranges for the analytes and matrices, and the correlation coefficients (R2) exceeded 0.99 for all the matrices.


Assuntos
Cromatografia Líquida/métodos , Lipídeos/isolamento & purificação , Progestinas/análise , Espectrometria de Massas em Tandem/métodos , Animais , Calibragem , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Progestinas/farmacocinética
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