microcolumn liquid chromatography
liquid chromatography/mass spectrometry
Analytical Chemistry and Spectroscopy
Wiley InterScience Backfile Collection 1832-2000
Chemistry and Pharmacology
A temperature-programmed microcolumn liquid chromatography/mass spectrometry (LC/MS) system has been developed as a practical alternative to conventional solvent-programmed LC/MS. Good reproducibility of solute retention was achieved in a specially modified oven that permitted linear temperature programming between 40 and 100°C at rates of 0.1 to 0.5°C min-1. Through theoretical modelling studies performed under isocratic and isothermal conditions, the optimum separation under temperature-programmed conditions was rapidly and accurately predicted. This method enabled the complete resolution of saturated and unsaturated fatty acids in a fish oil dietary supplement with identification from their characteristic fragmentation patterns under electron-impact MS conditions. The mass spectra from the LC/MS system correlated very well with those from a standard reference library to facilitate spectral searching methods.
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