PMID- 36542787 OWN - NLM STAT- MEDLINE DCOM- 20230119 LR - 20231021 IS - 1520-6882 (Electronic) IS - 0003-2700 (Print) IS - 0003-2700 (Linking) VI - 95 IP - 2 DP - 2023 Jan 17 TI - Quantitative Bottom-Up Glycomic Analysis of Polysaccharides in Food Matrices Using Liquid Chromatography-Tandem Mass Spectrometry. PG - 1008-1015 LID - 10.1021/acs.analchem.2c03707 [doi] AB - Carbohydrates are the most abundant biomolecules in nature, and specifically, polysaccharides are present in almost all plants and fungi. Due to their compositional diversity, polysaccharide analysis remains challenging. Compared to other biomolecules, high-throughput analysis for carbohydrates has yet to be developed. To address this gap in analytical science, we have developed a multiplexed, high-throughput, and quantitative approach for polysaccharide analysis in foods. Specifically, polysaccharides were depolymerized using a nonenzymatic chemical digestion process followed by oligosaccharide fingerprinting using high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-QTOF-MS). Both label-free relative quantitation and absolute quantitation were done based on the abundances of oligosaccharides produced. Method validation included evaluating recovery for a range of polysaccharide standards and a breakfast cereal standard reference material. Nine polysaccharides (starch, cellulose, beta-glucan, mannan, galactan, arabinan, xylan, xyloglucan, chitin) were successfully quantitated with sufficient accuracy (5-25% bias) and high reproducibility (2-15% CV). Additionally, the method was used to identify and quantitate polysaccharides from a diverse sample set of food samples. Absolute concentrations of nine polysaccharides from apples and onions were obtained using an external calibration curve, where varietal differences were observed in some of the samples. The methodology developed in this study will provide complementary polysaccharide-level information to deepen our understanding of the interactions of dietary polysaccharides, gut microbial community, and human health. FAU - Bacalzo, Nikita P Jr AU - Bacalzo NP Jr AUID- ORCID: 0000-0002-6253-6340 AD - Department of Chemistry, University of California horizontal line Davis, Davis, California 95616, United States. FAU - Couture, Garret AU - Couture G AUID- ORCID: 0000-0002-8947-4354 AD - Department of Chemistry, University of California horizontal line Davis, Davis, California 95616, United States. FAU - Chen, Ye AU - Chen Y AUID- ORCID: 0000-0002-6379-1968 AD - Department of Chemistry, University of California horizontal line Davis, Davis, California 95616, United States. FAU - Castillo, Juan J AU - Castillo JJ AUID- ORCID: 0000-0001-9680-5273 AD - Department of Chemistry, University of California horizontal line Davis, Davis, California 95616, United States. FAU - Phillips, Katherine M AU - Phillips KM AD - Virginia Tech, Blacksburg, Virginia 24061, United States. FAU - Fukagawa, Naomi K AU - Fukagawa NK AD - Beltsville Human Nutrition Research Center, USDA Agricultural Research Service, Beltsville, Maryland 20705, United States. FAU - Lebrilla, Carlito B AU - Lebrilla CB AUID- ORCID: 0000-0001-7190-5323 AD - Department of Chemistry, University of California horizontal line Davis, Davis, California 95616, United States. AD - Department of Biochemistry and Molecular Medicine, University of California horizontal line Davis, Davis, California 95616, United States. LA - eng GR - R01 DK124193/DK/NIDDK NIH HHS/United States PT - Journal Article PT - Research Support, N.I.H., Extramural PT - Research Support, U.S. Gov't, Non-P.H.S. DEP - 20221221 PL - United States TA - Anal Chem JT - Analytical chemistry JID - 0370536 RN - 0 (Polysaccharides) RN - 0 (Oligosaccharides) SB - IM MH - Humans MH - *Tandem Mass Spectrometry/methods MH - Reproducibility of Results MH - *Glycomics MH - Polysaccharides/chemistry MH - Chromatography, Liquid/methods MH - Oligosaccharides/chemistry MH - Chromatography, High Pressure Liquid/methods PMC - PMC9850401 COIS- The authors declare no competing financial interest. EDAT- 2022/12/22 06:00 MHDA- 2023/01/20 06:00 PMCR- 2023/01/19 CRDT- 2022/12/21 15:02 PHST- 2022/12/22 06:00 [pubmed] PHST- 2023/01/20 06:00 [medline] PHST- 2022/12/21 15:02 [entrez] PHST- 2023/01/19 00:00 [pmc-release] AID - 10.1021/acs.analchem.2c03707 [doi] PST - ppublish SO - Anal Chem. 2023 Jan 17;95(2):1008-1015. doi: 10.1021/acs.analchem.2c03707. Epub 2022 Dec 21.