Chromatographic Considerations and Maltitol Interference in Dietary Fiber Analysis
Year: 2026
Type: article
Abstract: BACKGROUND: AOAC 2017.16 and AOAC 2022.01 are CODEX Type I methods for total dietary fiber (TDF) that integrate enzymatic-gravimetric steps with high-performance liquid chromatography (HPLC) quantification of low molecular weight soluble dietary fiber (SDFS). As implementation expands, chromatography-related limitations and matrix-specific interferences can affect SDFS determination. OBJECTIVE: To evaluate performance of AOAC-recommended and alternative HPLC columns for DP2/DP3 boundary assignment across a broad carbohydrate set, and to investigate maltitol-associated interference leading to apparent SDFS overestimation in starch-containing matrixes. METHODS: Seventy-four carbohydrate standards (including oligosaccharides, polyols, and sugar alcohols) were analyzed in duplicate across five HPLC column configurations under AOAC 2017.16/2022.01 and AOAC 2009.01/2011.25 conditions. Column performance was scored by correct peak-area assignment relative to the maltose demarcation. Maltitol interference was assessed using food products formulated with/without maltitol and mixtures of maltitol (and other polyols) with wheat starch or wheat flour using scaled AOAC 2017.16 and AOAC 2001.03 procedures. RESULTS: Across 74 analytes, SugarPak (Waters) provided the highest overall assignment accuracy, with a two-column series configuration scoring highest. Maltitol alone could be excluded by adjusting the DP2/DP3 demarcation; however, maltitol combined with glucose-based polymers produced an additional peak area in the SDFS region, yielding up to ∼8% apparent SDFS overestimation in wheat starch mixtures. CONCLUSIONS: Chromatographic selection materially affects DP2/DP3 assignment for SDFS quantification. Maltitol can cause matrix-dependent artifactual SDFS in starch-containing test materials, suggesting formation of low-molecular-weight species during enzymatic processing. Guidance on column equivalency would strengthen AOAC dietary fiber methodology, and further work is warranted to further investigate maltitol interaction with glucose-based polymers during TDF analysis. HIGHLIGHTS: SugarPak showed best DP2/DP3 peak-area assignment across 74 standards. Several analytes elute at/near the demarcation depending on column configuration. Maltitol + starch matrixes can generate artifactual SDFS and inflate TDF.
Source: Journal of AOAC International
Authors: Tadas Kargelis, Zhen K Lam, David Mangan
Language: English
Subfield: Nutrition and Dietetics
Field: Nursing
Domain: Health Sciences
SDG: Zero hunger
Open Access status: hybrid
Estimated APC paid: $1,868
OpenAlex ID: W7133120620