Layer-by-layer functionalized porous Zinc sulfide nanospheres-based solid-phase extraction combined with liquid chromatography time-of-flight/mass and gas chromatography-mass spectrometry for the specific enrichment and identification of alkaloids from Cr

• ZnS nanospheres as SPE sorbents were developed for the specific enrichment and identification of alkaloids from Crinum asiaticum var. sinicum.
• The ZnS-based sorbents were prepared by the amidation reaction of poly-(acrylic acid) homopolymer with amino groups onto the porus ZnS nanospheres.
• The developed SPE protocol could improve the extraction efficiency and selectivity for the alkaloids via the electrostatic interaction.
• Tandem LC-TOF/MS spectrometry presented that the most all of the twenty-three main peaks in fraction from the SPE could be inferred as alkaloids.
• Seven alkaloids including two new found chemical entities were directly identified from their GC-MS spectra.

The current widely utilized polymer or C8, C18 end-capped material-based sorbents for solid-phase extraction could not capture alkaloids well only based on “like dissolves like” principle. In this paper, a layer-by-layer functionalized porous Zinc sulfide nanospheres-based solid-phase extraction (SPE) combined with liquid chromatography time-of-flight/mass spectrometry (LC-TOF/MS) and gas chromatography-mass spectrometry (GC-MS) was developed for the specific enrichment and identification of alkaloids from complex matrixes, Crinum asiaticum var. sinicum crude extracts. The functionalized porous Zinc sulfide nanospheres were prepared by the amidation reaction of poly-(acrylic acid) (PAA) homopolymer with amino groups onto the porous ZnS nanospheres. Tandem LC-TOF/MS spectrometry presented that the almost all of the twenty-three main peaks in elution fraction from the SPE could be inferred as alkaloids with ion of mass according to the nitrogen rule and hit formula with Peak View1.2@software from AB SCIEX, and seven alkaloids including two new found chemical entities were directly identified from their GC-MS spectra and retention indices. We believe that this SPE protocol can also be utilized in the future to selectively enrich alkaloids from extracts of other plant species.

Figure optionsDownload as PowerPoint slide