The use of g.l.c. coupled to mass spectrometry to separate and sequence permethylated acetyl- and trifluoroacetyl-peptides in a single operation is described. Both electron impact and chemical ionization were used to induce fragmentation, and the latter was found to be more sensitive. Chromatographic retention data are presented which suggest that peptide derivatives of molecular weight of at least 750 are accessible to the technique. The application of our methods to the determination of the primary sequence of proteins is discussed.

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