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Poly(ethylene glycol) functionalization of monolithic poly(divinyl benzene) for improved miniaturized solid phase extraction of protein-rich samples


Candish, E and Khodabandeh, A and Gaborieau, M and Rodemann, T and Shellie, RA and Gooley, AA and Hilder, EF, Poly(ethylene glycol) functionalization of monolithic poly(divinyl benzene) for improved miniaturized solid phase extraction of protein-rich samples, Analytical and Bioanalytical Chemistry, 409, (8) pp. 2189-2199. ISSN 1618-2642 (2017) [Refereed Article]

Copyright Statement

Copyright Springer-Verlag Berlin Heidelberg 2017

DOI: doi:10.1007/s00216-016-0164-y


Non-specific protein adsorption on hydrophobic solid phase extraction (SPE) adsorbents can reduce the efficacy of purification. To improve sample clean-up, poly(divinyl benzene) (PDVB) monoliths grafted with hydrophilic polyethylene glycol methacrylate (PEGMA) were developed. Residual vinyl groups (RVGs) of the PDVB were employed as anchor points for PEGMA grafting. Two PEGMA monomers, Mn 360 and 950, were compared for graft solutions containing 5–20% monomer. Protein binding was qualitatively screened using fluorescently labeled human serum albumin (HSA) to determine optimal PEGMA concentration. The fluorescent signal of PDVB was reduced for PDVB-g-PEGMA360 (10%) and PDVB-g-PEGMA950 (20%). The PEGMA content (w/w%) was quantified by solid state 1H NMR to be 29.9 ± 1.6% for PDVB-g-PEGMA360 and 7.7 ± 1.2% for PDVB-g-PEGMA950. To assess adsorbent performance breakthrough curves for PDVB, PDVB-g-PEGMA360 and PDVB-g-PEGMA950 were compared. The breakthrough volume (VB) and shape of the curve for PDVB-g-PEGMA950 were maintained relative to PDVB (2.3 and 2.8 mL, respectively). A reduced VB of 0.5 mL and shallow breakthrough curve indicated PDVB-g-PEGMA360 was not suitable for SPE. A high ibuprofen recovery of 92 ± 0.30 and 78 ± 0.93% was seen for PDVB and PDVB-g-PEGMA950, respectively. Protein adsorption was reduced from 31 ± 2.41 to 12 ± 0.49% for PDVB and PDVB-g-PEGMA950, respectively. SPE of ibuprofen from plasma was compared for PDVB and PDVB-g-PEGMA950 by at-line electrospray ionization mass spectrometry (ESI-MS). PDVB-g-PEGMA950 demonstrated a threefold increase in assay sensitivity indicating a superior analyte purification.

Item Details

Item Type:Refereed Article
Keywords:sample preparation, porous polymer monolith, solid phase extraction, grafting, biocompatible
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Candish, E (Ms Esme Candish)
UTAS Author:Khodabandeh, A (Mr Aminreza Khodabandeh)
UTAS Author:Rodemann, T (Dr Thomas Rodemann)
UTAS Author:Shellie, RA (Professor Robert Shellie)
UTAS Author:Gooley, AA (Dr Andrew Gooley)
UTAS Author:Hilder, EF (Professor Emily Hilder)
ID Code:119048
Year Published:2017
Web of Science® Times Cited:14
Deposited By:Central Science Laboratory
Deposited On:2017-07-25
Last Modified:2022-08-26

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