Solid-Phase Extraction Approaches for Improving Oligosaccharide and Small Peptide Identification with Liquid Chromatography-High-Resolution Mass Spectrometry: A Case Study on Proteolyzed Almond Extract

Yu Ping Huang, Randall C. Robinson, Fernanda Furlan Goncalves Dias, Juliana Maria Leite Nobrega de Moura Bell, Daniela Barile

Research output: Contribution to journalArticlepeer-review

13 Scopus citations

Abstract

Reverse-phase solid-phase extraction (SPE) is regularly used for separating and puri-fying food-derived oligosaccharides and peptides prior to liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. However, the diversity in physicochemical properties of peptides may prevent the complete separation of the two types of analytes. Peptides present in the oligosaccharide fraction not only interfere with glycomics analysis but also escape peptidomics analysis. This work evaluated different SPE approaches for improving LC-MS/MS analysis of both oligosaccharides and peptides through testing on peptide standards and a food sample of commercial interest (proteolyzed almond extract). Compared with conventional reverse-phase SPE, mixed-mode SPE (reverse-phase/strong cation exchange) was more effective in retaining small/hydrophilic peptides and capturing them in the high-organic fraction and thus allowed the identification of more oligosaccharides and dipeptides in the proteolyzed almond extract, with satisfactory MS/MS confir-mation. Overall, mixed-mode SPE emerged as the ideal method for simultaneously improving the identification of food-derived oligosaccharides and small peptides using LC-MS/MS analysis.

Original languageEnglish (US)
Article number340
JournalFoods
Volume11
Issue number3
DOIs
StatePublished - Feb 1 2022
Externally publishedYes

Bibliographical note

Funding Information:
Funding: Funding for this study was made possible by the U.S. Department of Agriculture’s (USDA) Agricultural Marketing Service through grant AM170100XXXXG011 and USDA NIFA project CA−DFST-2187-H. Its contents are solely the responsibility of the authors and do not necessarily represent the official views of the USDA.

Publisher Copyright:
© 2022 by the authors. Licensee MDPI, Basel, Switzerland.

Keywords

  • Glycomics
  • LC-MS/MS
  • Mixed-mode solid-phase extraction
  • Peptidomics
  • Protein hydrolysates
  • Sample preparation

PubMed: MeSH publication types

  • Journal Article

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