Application of liquid chromatography-two-dimensional nuclear magnetic resonance spectroscopy using pre-concentration column trapping and liquid chromatography-mass spectrometry for the identification of degradation products in stressed commercial amlodipine maleate tablets

Journal of Chromatography. a
Tomonori MurakamiFumiyo Kusu

Abstract

Application of the HPLC hyphenated techniques of LC-two-dimensional (2D) NMR using pre-concentration column trapping and LC-MS was demonstrated by the identification of two major degradation products, DP-1 and DP-2, in stressed commercial tablets of amlodipine maleate. The molecular formulas were estimated by LC-MS. Sample pre-concentration by column trapping was conducted to obtain adequate 2D-NMR signals by reducing the peak widths of the degradation products and making sure that the maximum amount of each component was inside the flow cell for NMR detection. Double-quantum filtered correlation spectroscopy (DQF-COSY) was applied to identify DP-1 as beta-N-lactosylamlodipine by suppressing the residual water signal without affecting the sample signal and by measuring the coupling constant of the lactose anomeric proton. Heteronuclear multiple bond coherence spectroscopy (HMBC) was applied to characterize DP-2 as an aspartic acid derivative of amlodipine by detecting long-range CH correlations. The chemical structures of the degradation products could be successfully elucidated unambiguously without an isolation process.

References

Jul 8, 1991·Ugeskrift for laeger·O L Pedersen, P Schroeder
May 17, 2005·Biochimica Et Biophysica Acta·Mikhail D LinetskyOgnyan O Argirov
May 6, 2006·Rapid Communications in Mass Spectrometry : RCM·John GibbonsRichard Pike

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Citations

Apr 1, 2011·Journal of Pharmaceutical Sciences·Changkang PanMichael Motto
May 12, 2017·Biomedical Chromatography : BMC·Purushotham Reddy ChallaNarayana Rao K M V
Jan 9, 2017·Journal of Pharmaceutical and Biomedical Analysis·Tarun HandaSaranjit Singh
May 4, 2018·Rapid Communications in Mass Spectrometry : RCM·C Purna ChanderR Srinivas
Mar 24, 2009·The Analyst·Suwatchai JarussophonYasuo Konishi

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