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Gewählte Publikation:

Zweckmair, T; Becker, M; Ahn, K; Hettegger, H; Kosma, P; Rosenau, T; Potthast, A; .
(2014): A novel method to analyze the degree of acetylation in biopolymers.
J Chromatogr A. 2014; 1372C:212-220 FullText FullText_BOKU

Abstract:
A novel approach to measure the degree of acetylation in biopolymers applying a combination of Zemplen-deacetylation by sodium methanolate and GC-MS methodology is introduced. The development focuses on very low limits of detection to cover also samples with extremely low degrees of acetylation which hitherto eluded accurate determination. Free acetic acid or inorganic acetates, often present in biopolymer samples, do not disturb the quantification. Two techniques to measure the Zemplen-released methyl acetate were comparatively assessed, direct injection of the liquid phase and a SPME-based approach, the former being more straightforward, but being inferior to the latter in sensitivity. By applying isotopically labeled methyl acetate released from 4-O-(C-13(2)-acetyl)-vanillin as the internal standard, influences, such as varying moisture contents, are corrected, improving the overall method reliability to a large extent. The combination of Zemplen-release of acetyl groups in biopolymers as methyl acetate, in connection with its accurate quantification by SPME GC MS, was found to be the method of choice for routine, yet very accurate analysis of a wide range of acetylation degrees of biopolymers, showing satisfying analytical parameters along with easy handling and widest applicability. Limit of detection for acetylated cellulose samples is 0.09 nmol/mg, for hemicellulose samples 0.48 nmol/mg. (C) 2014 Elsevier B.V. All rights reserved.
Autor*innen der BOKU Wien:
Ahn Kyujin
Becker Manuel
Hettegger Hubert
Kosma Paul
Potthast Antje
Rosenau Thomas
Zweckmair Thomas
BOKU Gendermonitor:


Find related publications in this database (Keywords)
Carbohydrates
Degree of acetylation
GC-MS
Methyl acetate
Polysaccharides
SPME
Zemplen transesterification


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