title: The characterization of crude products from solid-phase peptide synthesis by mu-HPLC/fast atom bombardment mass spectrometry.
abstract: Crude product mixtures from the solid-phase synthesis of a series of peptides were analyzed by on-line packed, fused silica column mu-HPLC/Continuous Flow Fast Atom Bombardment Mass Spectrometry (mu-HPLC/CF-FABMS). The technique is superior to the direct FAB analysis of crude product mixtures since competitive ionization and suppression effects are not generally observed. Positive correlation between a chromatographic peak and the desired synthetic product may be obtained. An accurate assessment of peptide deprotection can be made without ambiguity arising from the MS fragmentation of the more labile t-butyl and BOC protecting groups used in FMOC-based solid-phase peptide synthesis strategies. mu-HPLC combined with in-line UV detection and MS analysis allows the use of minimum sample and injection volumes, typically 10-50 pmol contained in 0.2-0.5 microliters.
authors.affiliation: Boehringer Ingelheim Pharmaceuticals, Inc., Ridgefield, CT 06877.
authors.forename: K
authors.initials: K
authors.lastname: McKellop
authors.forename: W
authors.initials: W
authors.lastname: Davidson
authors.forename: G
authors.initials: G
authors.lastname: Hansen
authors.forename: D
authors.initials: D
authors.lastname: Freeman
authors.forename: P
authors.initials: P
authors.lastname: Pallai
mesh_terms: D000595:Amino Acid Sequence; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D008969:Molecular Sequence Data; D009842:Oligopeptides / Q000032:analysis* / Q000138:chemical synthesis / Q000737:chemistry; D010456:Peptides, Cyclic / Q000032:analysis / Q000138:chemical synthesis / Q000737:chemistry; D016339:Spectrometry, Mass, Fast Atom Bombardment / Q000379:methods*
chemical_list: D009842:Oligopeptides; D010456:Peptides, Cyclic