title: Development and Application of a Novel SPE-Method for Bioassay-Guided Fractionation of Marine Extracts.
abstract: The biological diversity of marine habitats is a unique source of chemical compounds with potential use as pharmaceuticals, cosmetics and dietary supplements. However, biological screening and chemical analysis of marine extracts pose specific technical constraints and require adequate sample preparation. Here we report an improved method on Solid Phase Extraction (SPE) to fractionate organic extracts containing high concentration of salt that hampers the recovery of secondary metabolites. The procedure uses a water suspension to load the extracts on a poly(styrene-divynylbenzene)-based support and a stepwise organic solvent elution to effectively desalt and fractionate the organic components. The novel protocol has been tested on MeOH-soluble material from three model organisms (Reniera sarai, Dendrilla membranosa and Amphidinium carterae) and was validated on a small panel of 47 marine samples, including sponges and protists, within discovery programs for identification of immuno-stimulatory and anti-infective natural products.
authors.affiliation: Bio-Organic Chemistry Unit, Institute of Biomolecular Chemistry-CNR, Via Campi Flegrei 34, Pozzuoli, Naples 80078, Italy. acutignano@icb.cnr.it.
authors.forename: Adele
authors.initials: A
authors.lastname: Cutignano
authors.affiliation: Bio-Organic Chemistry Unit, Institute of Biomolecular Chemistry-CNR, Via Campi Flegrei 34, Pozzuoli, Naples 80078, Italy. nuzzo.genoveffa@icb.cnr.it.
authors.forename: Genoveffa
authors.initials: G
authors.lastname: Nuzzo
authors.affiliation: Marine Biotechnology Laboratory, Integrative Marine Ecology Department, Stazione Zoologica Anton Dohrn, Villa Comunale, Naples 80121, Italy. ianora@szn.it.
authors.forename: Adrianna
authors.initials: A
authors.lastname: Ianora
authors.affiliation: Bio-Organic Chemistry Unit, Institute of Biomolecular Chemistry-CNR, Via Campi Flegrei 34, Pozzuoli, Naples 80078, Italy. elvira.luongo@icb.cnr.it.
authors.forename: Elvira
authors.initials: E
authors.lastname: Luongo
authors.affiliation: Marine Biotechnology Laboratory, Integrative Marine Ecology Department, Stazione Zoologica Anton Dohrn, Villa Comunale, Naples 80121, Italy. romano@szn.it.
authors.forename: Giovanna
authors.initials: G
authors.lastname: Romano
authors.affiliation: Bio-Organic Chemistry Unit, Institute of Biomolecular Chemistry-CNR, Via Campi Flegrei 34, Pozzuoli, Naples 80078, Italy. carmen.gallo@icb.cnr.it.
authors.forename: Carmela
authors.initials: C
authors.lastname: Gallo
authors.affiliation: Marine Biotechnology Laboratory, Integrative Marine Ecology Department, Stazione Zoologica Anton Dohrn, Villa Comunale, Naples 80121, Italy. clementina.sansone@szn.it.
authors.forename: Clementina
authors.initials: C
authors.lastname: Sansone
authors.affiliation: GSK Vaccines s.r.l., via Fiorentina 1, Siena 53100, Italy. susanna.x.aprea@gsk.com.
authors.forename: Susanna
authors.initials: S
authors.lastname: Aprea
authors.affiliation: GSK Vaccines s.r.l., via Fiorentina 1, Siena 53100, Italy. francesca.x.mancini@gsk.com.
authors.forename: Francesca
authors.initials: F
authors.lastname: Mancini
authors.affiliation: GSK Vaccines s.r.l., via Fiorentina 1, Siena 53100, Italy. ugo.x.d'oro@gsk.com.
authors.forename: Ugo
authors.initials: U
authors.lastname: D'Oro
authors.affiliation: Bio-Organic Chemistry Unit, Institute of Biomolecular Chemistry-CNR, Via Campi Flegrei 34, Pozzuoli, Naples 80078, Italy. afontana@icb.cnr.it.
authors.forename: Angelo
authors.initials: A
authors.lastname: Fontana
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000737:chemistry / Q000494:pharmacology; D001419:Bacteria / Q000187:drug effects; D001681:Biological Assay; D005591:Chemical Fractionation / Q000379:methods*; D004141:Dinoflagellida / Q000737:chemistry*; D058086:Microalgae / Q000502:physiology; D011161:Porifera / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D000900:Anti-Bacterial Agents
keywords: SPE fractionation methods; bioactive marine natural products; drug discovery