Microchimica Acta

, 186:164 | Cite as

Bi-functionalized mesostructured silicas as reversed-phase/strong anion-exchange sorbents. Application to extraction of polyphenols prior to their quantitation by UHPLC with ion-trap mass spectrometry detection

  • Natalia Casado
  • Damián Pérez-Quintanilla
  • Sonia Morante-Zarcero
  • Isabel SierraEmail author
Original Paper


Hybrid mesostructured silicas with wormhole-like pore structure were synthesized and bi-functionalized with n-octyl (C8) and quaternary ammonium (NR4+) groups to obtain new sorbent materials for dispersive solid-phase extraction (dSPE) of polyphenols. Due to their nature of being both a reversed-phase and a strong anion-exchanger, the materials display mixed-mode retention mechanism. During the synthesis, the functionalization conditions were varied to obtain materials with different functionalization degree. The resulting materials (denoted as HMS-RPC8-SAX-1, HMS-RPC8-SAX-2 and HMS-RPC8-SAX-3) show high surface area, wormhole-like framework and controlled pore size. They were evaluated for multicomponent extraction of 22 polyphenols, including phenolic acids, flavonoids and stilbenes, from spiked juice samples. The sample extracts were analyzed by ultra-high performance liquid chromatography coupled to ion-trap tandem mass spectrometry. The adsorption capability, the amount of sorbent, the eluent and the elution volume were optimized. Best performance was achieved by using HMS-RPC8-SAX-2, which is the material with the highest fraction of NR4+ groups. This material has a large extraction capability and provides high recovery values of the target analytes (70–101%) as a result of its hydrophobic and anion-exchange interactions. The detection limits for polyphenols in juice range from 1 to 560 ng mL−1.

Graphical abstract

Schematic presentation of dispersive solid-phase extraction of polyphenols from juice samples using a novel sorbent based on the bi-functionalization of mesostructured silica with n-octyl and quaternary ammonium groups, followed by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) analysis. Due to the sorbent nature of being both a reversed-phase and strong anion-exchanger, the material displays mixed mode retention mechanism that improves its extraction capability.


Dispersive solid-phase extraction Flavonoids Phenolic acids Stilbenes Juice Porous sorbents Quaternary ammonium groups Sample preparation 



Authors thank financial support from the Comunidad of Madrid and European funding from FEDER program (Project S2013/ABI-3028, AVANSECAL).

Compliance with ethical standards

The author(s) declare that they have no competing interests.

Supplementary material

604_2019_3267_MOESM1_ESM.docx (3.1 mb)
ESM 1 (DOCX 3220 kb)


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Copyright information

© Springer-Verlag GmbH Austria, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Departamento de Tecnología Química Ambiental, E.S.C.E.TUniversidad Rey Juan CarlosMadridSpain

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