title: Liquid chromatography-mass spectrometry approach for the characterization and purification of crude synthetic peptide hormones.
abstract: In this study, conditions for the optimal separation by LC-UV and characterisation by LC-ES-MS of crude mixtures generated during SPPS of several peptide hormones are compiled. The linear solvation energy relationship (LSER) methodology has been used to predict the retention of the target peptides and their side products and then to develop a separation LC methodology with applicability on both the analytical and preparative scale. Identification of these side products by LC-ES-MS analysis has been made on the basis of their calculated molecular masses. This method may be regarded as a key tool for the optimisation of the synthetic procedures and for complying with regulatory agencies' requirements before commercialisation of a safe and effective peptide-based pharmaceutical drug.
authors.affiliation: Department of Analytical Chemistry, University of Barcelona, Diagonal 647, 08028 Barcelona, Spain. vsanz@apolo.qui.ub.es
authors.forename: Victoria
authors.initials: V
authors.lastname: Sanz-Nebot
authors.forename: Fernando
authors.initials: F
authors.lastname: Benavente
authors.forename: Isabel
authors.initials: I
authors.lastname: Toro
authors.forename: José
authors.initials: J
authors.lastname: Barbosa
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D010084:Oxidation-Reduction; D036361:Peptide Hormones / Q000737:chemistry* / Q000302:isolation & purification*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet
chemical_list: D036361:Peptide Hormones