title: Rapid HILIC method with fluorescence detection using derivatization reaction utilizing o-phthaldialdehyde for determination of degradation product of aliskiren.
abstract: A rapid procedure based on direct extraction and HILIC separation of aliskiren (ALI) degradation product - 3-amino-2,2-dimethylpropanamide (ADPA) with fluorescence detection has been developed. The formation of ADPA from ALI under different conditions was studied. The evaluation of HILIC method robustness was performed using multifactorial experiments with fixed factors (one-level Plackett-Burman design). XBridge HILIC column with isocratic elution using mobile phase 10 mM K(2)HPO(4) pH 7.2-acetonitrile (26:74; v/v) was employed. Fluorescence detection after post column derivatization using o-phthaldialdehyde (OPA) reagent was performed at excitation and emission wavelength of 345 nm and 450 nm, respectively. The reported method has an advantage of a simple sample pre-treatment and quick and very sensitive measurement. The method was successfully applied for the analysis of commercially available ALI samples.
authors.affiliation: Zentiva, a.s. Praha, U Kabelovny 130, 102 37 Praha 10, Czech Republic. hplc@hplc.cz
authors.forename: Michal
authors.initials: M
authors.lastname: Douša
authors.forename: Jiří
authors.initials: J
authors.lastname: Břicháč
authors.forename: Jiří
authors.initials: J
authors.lastname: Svoboda
authors.forename: Robert
authors.initials: R
authors.lastname: Klvaňa
mesh_terms: D000577:Amides / Q000032:analysis* / Q000737:chemistry; D000596:Amino Acids / Q000032:analysis*; D000959:Antihypertensive Agents / Q000032:analysis* / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods*; D005650:Fumarates / Q000032:analysis* / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods; D012680:Sensitivity and Specificity; D013050:Spectrometry, Fluorescence / Q000379:methods; D013997:Time Factors; D009764:o-Phthalaldehyde / Q000737:chemistry
chemical_list: C575427:3-amino-2,2-dimethylpropanamide; D000577:Amides; D000596:Amino Acids; D000959:Antihypertensive Agents; D005650:Fumarates; C446481:aliskiren; D009764:o-Phthalaldehyde