Separation and detection of 4-hexadecylaniline maltooligosaccharide derivatives with packed capillary liquid chromatography-frit fast atom bombardment-mass spectrometry.

A LC-MS method is under development for the separation and detection of mixtures of native glycolipids and of oligosaccharide derivatives. The LC system is based on slurry-packed capillary columns. Frit fast atom bombardment (frit-FAB) is used as the LC-MS interface and ionisation technique and the column is connected to the frit via a 50 microns I.D. fused-silica capillary liner. Post column addition of matrix is achieved using a 50 microns I.D. fused-silica capillary liner with 2.5% (v/v) matrix solution. The two liners are joined through a septum and end side by side against the frit. The detection limit was found to be less than 1 pmole in the negative ion mode. A mixture of tetra to deca maltooligosaccharides reductively aminated with 4-hexadecylaniline (M4-10-HDA) was separated on a straight phase silica column using gradient elution.