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
Journal
Foods
Journal Volume
11
Journal Issue
3
Start Page
340
Date Issued
2022-01-25
Author(s)
Randall C. Robinson
Fernanda Furlan Goncalves Dias
Juliana Maria Leite Nobrega de Moura Bell
Daniela Barile
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.
Subjects
Glycomics
LC-MS/MS
Mixed-mode solid-phase extraction
Peptidomics
Protein hydrolysates
Sample preparation
Type
journal article