2D-HSQC-NMR-Based Screening of Feruloylated Side-Chains of Cereal Grain Arabinoxylans
Arabinoxylans of commelinid monocots are characterized by high contents of ferulic acid that is incorporated into arabinose-bearing side-chains of varying complexity. Species-related differences in the feruloylated side-chain profiles of grain arabinoxylans are observed and lead to differences in ar...
Saved in:
Published in | Frontiers in plant science Vol. 13; p. 951705 |
---|---|
Main Authors | , |
Format | Journal Article |
Language | English |
Published |
Frontiers Media S.A
07.07.2022
|
Subjects | |
Online Access | Get full text |
Cover
Loading…
Summary: | Arabinoxylans of commelinid monocots are characterized by high contents of ferulic acid that is incorporated into arabinose-bearing side-chains of varying complexity. Species-related differences in the feruloylated side-chain profiles of grain arabinoxylans are observed and lead to differences in arabinoxylan functionality. Here, a semi-quantitative assay based on
1
H-
13
C-correlation NMR spectroscopy (HSQC experiment) was developed to profile feruloylated side-chains of cereal grain arabinoxylans. Following acidic liberation of the feruloylated side-chains from the xylan backbone and a clean-up step using C18 solid phase extraction, the feruloylated oligosaccharides FA (5-
O
-
trans
-feruloyl-L-arabinofuranose), FAX (β-
d
-xylopyranosyl-(1 → 2)-5-
O
-
trans
-feruloyl-
l
-arabinofuranose) and FAXG (α-
l
-galactopyranosyl-(1 → 2)-β-
d
-xylopyranosyl-(1 → 2)-5-
O
-
trans
-feruloyl-
l
-arabinofuranose) were analyzed by HSQC-NMR. Marker signals were identified for each compound, and experimental conditions such as solvent and internal standard as well as measurement and processing conditions were optimized for a semi-quantitative determination. The approach was validated with respect to accuracy, precision, limit of detection, and limit of quantification. The newly developed approach was applied to several cereal samples including oats, popcorn maize, wheat, and wild rice. Data were compared to an HPLC-DAD/MS approach published earlier by our group, demonstrating that the results of the HSQC approach were comparable to the more time-consuming and technically more challenging HPLC-DAD/MS method. |
---|---|
Bibliography: | ObjectType-Article-1 SourceType-Scholarly Journals-1 ObjectType-Feature-2 content type line 23 Edited by: Jinsong Bao, Zhejiang University, China This article was submitted to Crop and Product Physiology, a section of the journal Frontiers in Plant Science Reviewed by: Amparo Jimenez Quero, Royal Institute of Technology, Sweden; Kedar Sharma, National Institute of Environmental Health Sciences (NIH), United States |
ISSN: | 1664-462X 1664-462X |
DOI: | 10.3389/fpls.2022.951705 |