The use of preparative high performance liquid chromatography with tandem mass spectrometric directed fraction collection for the isolation and characterisation of drug metabolites in urine by nuclear magnetic resonance spectroscopy and liquid chromatography sequential mass spectrometry
Rs. Plumb et al., The use of preparative high performance liquid chromatography with tandem mass spectrometric directed fraction collection for the isolation and characterisation of drug metabolites in urine by nuclear magnetic resonance spectroscopy and liquid chromatography sequential mass spectrometry, RAP C MASS, 13(10), 1999, pp. 845-854
Preparative high performance liquid chromatography (HPLC) coupled to tandem
mass spectrometry has been used successfully for the isolation of several
drug metabolites from urine. Nuclear magnetic resonance (NMR) spectroscopy
has been employed to determine the exact chemical structure of these metabo
lites. The use of preparative HPLC has allowed the isolation of relatively
large quantities of drug metabolites (>0.5 mg) allowing insensitive, inform
ation-rich NMR experiments such as NOE, HMBC and HMQC to be performed. The
coupling of the ion-trap mass spectrometer, operating in automatic MS/MS mo
de, to preparative HPLC allows the simultaneous collection and mass spectro
metric analysis of eluting analytes to be performed, thus allowing the posi
tion of fractions containing drug-related material to be identified very ra
pidly. Copyright (C) 1999 John Wiley & Sons, Ltd.