This investigation describes an integrated workflow for the parallel extraction and recovery of polyphenols and phytosterols from Pinot noir grape seeds. Using (E)-resveratrol and stigmasterol as exemplars, the approach employs two different molecular imprinted polymers in tandem for the extraction of these compounds and their subsequent analysis by capillary high-performance liquid chromatography (capHPLC) interfaced with electrospray ionisation tandem mass spectrometry (ESI MS/MS). Information on the selectivity of the solid-phase extraction processes was obtained through analysis of the binding behaviour of (E)-resveratrol- and stigmasterol-imprinted polymers using structurally similar polyphenols or phytosterols with the extent of binding determined from the capHPLC-ion trap ESI MS/MS data.
View Article and Find Full Text PDFIn this investigation, application of linear solvent energy relationships (LSERs) and principal component analysis (PCA) methods have been employed to investigate the structure-retention dependencies of E-resveratrol analogues separated under different stationary and mobile phase conditions. To this end, the retention of 22 analogues have been determined with phenyl, diol, bidentate anchored C18 (BDC18) and Diamond Hydride™ C18 (DHC18) substituted silica hydride stationary phases under isocratic chromatographic conditions using mobile phases containing 0.1 (% v/v) formic acid and different acetonitrile or methanol contents from 10 to 90% (v/v) in 10% increments.
View Article and Find Full Text PDFA new class of efficient stationary phase has been investigated for use in the liquid chromatographic separation of low molecular weight analytes and high molecular weight biomolecules, based on the application of immobilised stimuli-responsive polymers (SRPs). To this end, two polymeric units, namely poly(2-dimethylaminoethyl methacrylate) (PDMAEMA) and poly(acrylic acid) (PAA) were tethered to a triazine core. The derived poly(2-dimethyl-aminoethyl methacrylate)-block-poly(acrylic acid) (PDMAEMA-b-PAA), as a diblock co-polymer, was then immobilised onto the surface of porous silica particles.
View Article and Find Full Text PDFThis investigation describes a general procedure for the selectivity mapping of molecularly imprinted polymers, using (E)-resveratrol-imprinted polymers as the exemplar, and polyphenolic compounds present in Pinot noir grape skin extracts as the test compounds. The procedure is based on the analysis of samples generated before and after solid-phase extraction of (E)-resveratrol and other polyphenols contained within the Pinot noir grape skins using (E)-resveratrol-imprinted polymers. Capillary reversed-phase high-performance liquid chromatography (RP-HPLC) and electrospray ionisation tandem mass spectrometry (ESI MS/MS) was then employed for compound analysis and identification.
View Article and Find Full Text PDFA semi-covalent imprinting strategy has been developed for the synthesis of molecularly-imprinted polymers specific for the fungal sterol, ergosterol, a biological precursor of vitamin D. This imprinting approach involved a novel post-synthesis cleavable monomer-template composite, namely ergosteryl methacrylate, and resulted in the formation of an imprinted polymer that selectively and efficiently recognized ergosterol through non-covalent interactions. The derived molecularly-imprinted polymer and the corresponding non-imprinted polymer were systematically evaluated for their selectivity towards ergosterol via static and dynamic binding studies using various ergosteryl esters (e.
View Article and Find Full Text PDF