HIGH-RESOLUTION CAPILLARY GAS-CHROMATOGRAPHY AND GAS-CHROMATOGRAPHY MASS-SPECTROMETRY OF PROTEIN AND NONPROTEIN AMINO-ACIDS, AMINO-ALCOHOLS, AND HYDROXYCARBOXYLIC ACIDS AS THEIR TERT-BUTYLDIMETHYLSILYL DERIVATIVES

A simple, single-step derivatization technique is presented for capill ary GC-FID and GC-MS separation and identification of common protein a nd non-protein constituents of natural peptides as their tert-butyldim ethylsilyl (TBDMS) derivatives. The tert-butyldimethylsilylation of mo re than sixty compounds was accomplished with high yields and a single peak observed for each component. The TBDMS derivatives of both the p rotein and non-protein substances, moreover, exhibit excellent separat ion on apolar capillary columns and can be resolved completely using a polydimethylsiloxane or 5 % phenyl polydimethylsiloxane column and, c omplementarily, a 50 % phenyl polydimethylsiloxane column. Retention d ata and molar responses of the TBDMS derivatives on the polydimethylsi loxane column are compiled. Direct coupling of the 5 % phenyl polydime thylsiloxane column to an ion trap mass spectrometer enabled fast sepa ration and identification of the investigated components, at nanomole to picomole levels, on the basis of retention and mass spectral data, The general usefulness of the method is demonstrated by research into new biologically active peptides isolated from entomopathogenic fungi.