Determination of Terpenoid Content in Pine by Organic Solvent Extraction and Fast-GC Analysis

Abstract

Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts from the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α-and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. Diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.Keywords: fast-gc, pyrolysis-molecular beam mass spectrometry, cell wall chemistry, renewable materials, biofuels, bioproducts, biomaterials inTrODUcTiOn Renewable chemicals, including fuels, solvents, fragrances, flavors, and pharmaceutical compounds, can be generated or extracted from renewable biomass sources. Many types of compounds can be generated from different components of the biomass, e.g., ethanol from the carbohydrate fraction or biodiesel from the lipid components in biomass. Other biomass components, including lignin and oleoresin excretions from conifers, have also been used as a source of renewable chemicals. For example, pine oleoresin is used to generate turpentine, a solvent and source of synthetic platform chemicals such as α-pinene (Palmer, 1943;Beglinger, 1958). Terpenoids, naturally occurring organic compounds derived from isoprene units, are the primary constituents of pine oleoresin (Palmer, 1943;Bohlmann and Keeling, 2008;Rodrigues-Corrêa et al., 2012). Monoterpenes (C10), sesquiterpenes (C15), and diterpenoid resin acids (C20), the main terpenoids found in pine oleoresin, are a Abbreviations: BSTFA, N,O-Bis(trimethylsilyl)trifluoroacetamide; GC/FID, gas chromatography/flame ionization detector; LTM MACH, low thermal mass modular accelerated column heater; PLW, pine lighter wood; PS, pine sapling; py-MBMS, pyrolysis-molecular beam mass spectrometry. valuable source of chemicals with many industrial applications (Beglinger, 1958;Martin et al., 2002;Monteiro and Veloso, 2004;Bohlmann and Keeling, 2008;Harvey et al., 2009; RodriguesCorrêa et al., 2012). Turpentine is composed of monoterpenes and is used in the flavor and fragrance industry (Bohlmann and Keeling, 2008;Rodrigues-Corrêa et al., 2012). Other uses for terpenoid compounds have been found in pharmaceutical, cosmetics, and po...

Body-size Scaling is Related to Gut Microbial Diversity, Metabolism and Dietary Niche of Arboreal Folivorous Flying Squirrels

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Allelopathic Effects of Common Landscape and Nursery Mulch Materials on Weed Control

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