Characterization of hydrothermally isolated xylan from beech wood by capillary electrophoresis with laser-induced fluorescence and mass spectrometry detection

Abstract

Hemicelluloses such as xylans play an increasing role as renewable raw materials for technological applications. The complex and variable composition of hemicelluloses requires powerful analytical techniques in order to assess their composition. In the present study, the neutral fraction of hydrothermally isolated xylan from beech wood was characterized by capillary electrophoresis with laserinduced fluorescence detection (CE-LIF) upon derivatization with 8-aminopyrene-1,3,6-trisulfonic acid. Reproducible separation of the xylo-oligosaccharides was achieved using a polyvinyl alcohol coated capillary and a 25 mM sodium acetate buffer, pH 4.75, as background electrolyte at an applied voltage of -30 kV. Intermediate precision expressed as relative standard deviation was below 2.0 % for migration times and below 10 % for relative peak areas except for the oligomers present at very low concentrations only. At the same time, derivatization conditions proved to be robust as well. Samples obtained by fractionation of the xylan were subsequently characterized by CE-LIF. In addition, capillary electrophoresis with mass spectrometry detection indicated the presence of small amounts of xylo-oligosaccharides containing additional sugar moieties such as 4-Omethylglucuronic acid. Moreover, minor components Electronic supplementary material The online version of this article (

Derivatisation for separation and detection in capillary electrophoresis (2012–2015)

“…Novel magnetic nano beads were used for sample preparation including in situ protein digestion, glycan capture, derivatisation and sample clean‐up. 1‐Aminopyrene‐3,6,8‐trisulfonic acid labelling has been found useful for cellulose analysis . Fernández de la Ossa et al.…”

“…This is the traditional derivatisation method which has been the most popular with 2/3 of all articles in this review . Pre‐capillary labelling offers advantages in terms of chemical freedom and handling of the reagent and analytes.…”

“…Derivatisation in CE is used to improve or enable detection by LIF, UV, chemiluminescence (CL), electrochemiluminescence (ECL), amperometric detection (AD), MS or contactless conductivity detection (C4D). During this review period, there were papers 18 on LIF (and LIF combined with other detectors) [, , ], 18 on UV (and UV combined with other detectors) [, , ], two on CL , one on ECL , two on AD , three on MS (and MS combined with other detectors) and two on C4D .…”