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- A methodological approach for the simultaneous quantification of glycerol and fatty acids from cork suberin in a single GC runPublication . V Marques, A; Pereira, HelenaIntroduction: Suberin, as part of plant protective barriers, is one of the most important natural polymers after cellulose and lignin. For a full elucidation of suberin structure the quantification of glycerol, fatty α,ω‐diacids and ω‐hydroxyacids, the major building blocks of suberin, is of primary importance. Glycerol is often lost in the most used analytical procedures or rarely determined by deficient or too laborious techniques. Objectives: Propose a simple, accessible and reliable methanolysis work‐up procedure for an accurate and simultaneous quantification of glycerol and suberin fatty monomers in the same GC run. Material and methods: Cork from Quercus suber L. was depolymerised by methanolysis. Glycerol was derivatised to an organic soluble form before the suberin monomers recovery in water/organic solvent partition. Gas chromatography flame ionisation detector (GC‐FID) response factors were determined for glycerol, ferulic acid and one for each fatty monomer substructure. Additionally, 1,2,4‐butanetriol and methyl nonadecanoate were used as internal standards. Results: The proposed experimental approach allowed the glycerol and all the fatty suberin monomers in the same GC run to be quantified accurately. Glycerol represented 30.6 area%, 14.2 mass% and 38.4 molar% of suberin and the COOH/OH groups ratio was 0.6:1 in the proposed experimental approach in contrast with 0.10 area% and COOH/OH ratio of 3:1 in the most used protocol. Furthermore, ω‐hydroxyacids/α,ω‐diacids mass ratio was 1:1 as opposed to an area ratio of 1.5:1. Conclusion: The proposed work‐up procedure revealed to be a reliable analytical tool for the complete analysis of suberin allowing the future knowledge to grow towards a better understanding of suberin structure throughout its range and variability.
- An extensive study on the chemical diversity of lipophilic extractives from Eucalyptus globulus woodPublication . Gominho, Jorge; Lourenço, Ana; Marques, António Velez; Pereira, HelenaThree mature Eucalyptus globulus trees with 40 years of age were studied at three height levels (0%, 35%, and 60% of total tree height) and at three radial regions (sapwood, inner and outer heartwood). The composition of lipophilic extracts was evaluated and an extensive list of 202 compounds was reported for the first time. The fatty acids were the major chemical family, representing 40.8% of the total compounds, followed by phytosterols (19.0%), aromatics (10.5%) and triterpenes (10.4%). Saturated fatty acids accounted for 74.2% of total compounds (C-16(:0), C-24(:0) and C-26(:0) were predominant), beta-Sitosteml and stigmastanol were the main sterols (80 and 7% respectively), while aromatics were mainly represented by syringic acid, 4-hydroxy-3,5-dimethoxybenzaldehyde, vanillic acid, and vanillin. The main triterpenes were asiatic and arjunolic acids.