Dataset of Arabinoxylan Quantification in Gluten-Free Cereals via HPAEC-PAD Based on Design of Experiments

Arabinoxylans (AXs) are important dietary fibers in the cell walls of monocotyledonous cereals, contributing to digestive health and improved food functionality. Despite their nutritional relevance, no standardized analytical method is currently available for the quantification of AXs in gluten-free (GF) cereals. This dataset supports a study investigating the influence of hydrolysis parameters on AX quantification in GF cereals (maize, rice, and oat) with differing AX content and nutritional characteristics, addressing matrix-related effects. The impact of trifluoroacetic acid (TFA) concentration (0.25–4 M), hydrolysis temperature (90–127 °C), and time (1–5 h) on hydrolysis efficiency was systematically evaluated. Among these parameters, temperature exhibited a markedly stronger effect compared to acid concentration and hydrolysis time. Using a design-of-experiments (DoE) approach, optimal hydrolysis conditions (2 M TFA, 103 °C, 2.4 h) were predicted to maximize AX yield while avoiding detectable monosaccharide degradation across all cereal varieties. These conditions were experimentally validated with deviations below 10%. An extensive validation confirmed the accuracy and robustness of the proposed unified method for AX quantification in gluten-free cereal matrices.