title: Development and application of C60-fullerene bound silica for solid-phase extraction of biomolecules.
abstract: Sample pretreatment is the most important procedure to remove the matrix for interfacing with mass spectrometry (MS). Additionally, for the samples with low concentration, the process of preconcentration is required before MS analysis. We have newly developed a solid-phase extraction stationary phase based on C60-fullerene covalently bound to silica for purification of biomolecules of different characteristics. Silica particles of different porosity are modified with aminopropyl linker and then covalently bound to C60-fullerenoacetic acid or C60-epoxyfullerenes. The developed materials have been successfully applied as an alternative to commercially available reversed-phase materials for solid-phase extraction. C60-fullerene silica is able to retain small and hydrophilic molecules like phosphopeptides, which can be easily lost by reversed-phase sorbents. The novel materials are applied for desalting and preconcentration of proteins and peptides, especially phosphopeptides. In addition, the C60-fullerene silica is applied for the solid-phase extraction of selected flavonoids with recoveries of approximately 99%. The recoveries are compared with the commercially available solid-phase extraction materials.
authors.affiliation: Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens University, Innrain 52a, 6020 Innsbruck, Austria.
authors.forename: Rainer M
authors.initials: RM
authors.lastname: Vallant
authors.forename: Zoltan
authors.initials: Z
authors.lastname: Szabo
authors.forename: Stefan
authors.initials: S
authors.lastname: Bachmann
authors.forename: Rania
authors.initials: R
authors.lastname: Bakry
authors.forename: Muhammad
authors.initials: M
authors.lastname: Najam-ul-Haq
authors.forename: Matthias
authors.initials: M
authors.lastname: Rainer
authors.forename: Nico
authors.initials: N
authors.lastname: Heigl
authors.forename: Christine
authors.initials: C
authors.lastname: Petter
authors.forename: Christian W
authors.initials: CW
authors.lastname: Huck
authors.forename: Günther K
authors.initials: GK
authors.lastname: Bonn
mesh_terms: D005419:Flavonoids / Q000032:analysis*; D037741:Fullerenes / Q000737:chemistry*; D015394:Molecular Structure; D010316:Particle Size; D010455:Peptides / Q000032:analysis*; D011506:Proteins / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012822:Silicon Dioxide / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization / Q000379:methods; D019265:Spectroscopy, Near-Infrared / Q000379:methods; D013499:Surface Properties
chemical_list: D005419:Flavonoids; D037741:Fullerenes; D010455:Peptides; D011506:Proteins; D012822:Silicon Dioxide; C069837:fullerene C60