Rapid HILIC method with fluorescence detection using derivatization reaction utilizing o-phthaldialdehyde for determination of degradation product of aliskiren

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• 作者：Michal Dou&scaron ; a ; ^hplc@hplc.cz ; ^{michal.dousa@seznam.cz} ; Ji艡&iacute ; B艡ichá ; 膷 ; Ji艡&iacute ; Svoboda ; Robert Klva艌a
• 关键词：Aliskiren ; HILIC ; 3-Amino-2 ; 2-dimethylpropanamide (ADPA) ; Degradation product ; Related substances
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2012
• 期刊代码：65_07317085
• 类别：ch
• 出版时间：July, 2012
• 卷：66
• 期：Complete
• 页码：359-364
• 文件大小：515 K

摘要

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 K₂HPO₄ 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.