Solid-phase microextraction-gas chromatography-mass spectrometry of biologically active substances in water samples

High-flow pneumatically assisted electrospray ionization mass spectrometry (ESI-MS) has been extensively used for the characterization and determination of peptides and peptide hormones available for biomedical research and therapeutic applications. The aim of this study was to optimize a method of characterization and determination of a mixture of peptide hormones with therapeutic interest by liquid chromatography (LC) coupled to ESI-MS. In this work the linear solvation energy relationship methodology was used in order to optimize the mobile phase to be used in the LC separation of the peptide hormone series and the operational parameters of the source and analyzer of ESI were also optimized to obtain the best signal stability and the highest sensitivity. To validate the proposed method for peptide hormone analysis, quality parameters were determined and satisfactory results were obtained. Likewise, the method detection limit was picomole level for most of the peptides employing selected-ion monitoring of the M+nH]n+ ions.