Temperature‐programmed microcolumn liquid chromatography/mass spectrometry

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Abstract
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.