Benchtop versus high field NMR: Comparable performance found for the molecular weight determination of lignin

  • Lignin is a promising renewable biopolymer being investigated worldwide as an environmentally benign substitute of fossil-based aromatic compounds, e.g. for the use as an excipient with antioxidant and antimicrobial properties in drug delivery or even as active compound. For its successful implementation into process streams, a quick, easy, and reliable method is needed for its molecular weight determination. Here we present a method using 1H spectra of benchtop as well as conventional NMR systems in combination with multivariate data analysis, to determine lignin’s molecular weight (Mw and Mn) and polydispersity index (PDI). A set of 36 organosolv lignin samples (from Miscanthus x giganteus, Paulownia tomentosa and Silphium perfoliatum) was used for the calibration and cross validation, and 17 samples were used as external validation set. Validation errors between 5.6% and 12.9% were achieved for all parameters on all NMR devices (43, 60, 500 and 600 MHz). Surprisingly, no significant difference in the performance of the benchtop and high-field devices was found. This facilitates the application of this method for determining lignin’s molecular weight in an industrial environment because of the low maintenance expenditure, small footprint, ruggedness, and low cost of permanent magnet benchtop NMR systems.

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Author:René Burger, Simon Lindner, Jessica Rumpf, Xuan Tung Do, Bernd W.K. Diehl, Matthias Rehahn, Yulia MonakhovaORCiD, Margit Schulze
DOI:https://doi.org/10.1016/j.jpba.2022.114649
ISBN:0731-7085
Parent Title (English):Journal of Pharmaceutical and Biomedical Analysis
Publisher:Elsevier
Place of publication:New York, NY
Document Type:Article
Language:English
Year of Completion:2022
Date of the Publication (Server):2022/11/07
Tag:Biomass; Chemometrics; Molecular weight determination; NMR; PLS-regression
Volume:212
Issue:Article number: 114649
Link:https://doi.org/10.1016/j.jpba.2022.114649
Zugriffsart:bezahl
Institutes:FH Aachen / Fachbereich Chemie und Biotechnologie
collections:Verlag / Elsevier