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Analytical Method Cluster Development for Comprehensive Characterisation of Suberinic Acids Derived from Birch Outer
Daniela Godina1, Raimonds Makars1,2, Aigars Paze1
1Biorefinery Laboratory, Latvian State Institute of Wood Chemistry, LV-1006 Riga, Latvia.
Molecules (Basel, Switzerland)
|March 11, 2023
Summary
Developing instrumental analytical methods is crucial for suberin characterization in biorefineries. This study optimized GC-MS and MALDI-Tof techniques to identify suberin
Area of Science:
- Biomass Valorization
- Polymer Chemistry
- Analytical Chemistry
Background:
- Suberin, a complex polyester biopolymer, presents challenges in accurate content determination in plant tissues.
- Developing robust analytical methods is essential for integrating suberin-derived products into biorefinery value chains.
Purpose of the Study:
- To optimize instrumental analytical methods for comprehensive suberin characterization.
- To identify the main monomeric units and structural components of suberin acid (SA).
Main Methods:
- Optimization of two Gas Chromatography-Mass Spectrometry (GC-MS) methods: direct silylation and silylation with prior depolymerization.
- Gel Permeation Chromatography (GPC) with Refractive Index (RI) and Multi-Angle Light Scattering (MALS) detectors (18-angle MALS preferred due to sample fluorescence).
- Matrix-Assisted Laser Desorption/Ionization-Time of Flight (MALDI-Tof) mass spectrometry for non-degraded suberin structure determination.
- Treatment of suberin acid (SA) with ferric chloride (FeCl3) to remove phenolic admixtures.
Main Results:
- GC-MS identified free monomeric units and, after depolymerization, the complete potential monomeric unit composition of SA.
- GPC analysis, particularly with an 18-angle MALS detector, determined the molar mass distribution of SA.
- MALDI-Tof analysis revealed octadecanedioic acid and 2-(1,3-dihydroxyprop-2-oxy)decanedioic acid as the primary monomeric units in the SA macromolecular structure.
- FeCl3 treatment reduced phenolic content and molecular weight of SA samples.
Conclusions:
- Optimized GC-MS and MALDI-Tof methods provide comprehensive characterization of suberin, enabling accurate analysis of its composition and structure.
- The identified monomeric units confirm the complex polyester nature of suberin and provide insights for its utilization in biorefineries.
- Advanced analytical techniques are vital for unlocking the full potential of suberin in industrial applications.
