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The aim of the study was to find appropriate non-chlorinated solvent systems for the extraction and separation of pure pinosylvin (PS) and pinosylvin monomethylether (PSMME) from Scots pine/Norway spruce wood residues. The extraction was performed in a pressurized solvent extractor and the purification and isolation of pure substances was done by flash chromatography. More precisely, pure PS was isolated via sequential flash chromatography in two repetitions in the gradient mode of the mobile phase, with cylcohexane (CX) and ethylacetate (EtOAc), beginning with 100% CX and ending up with 100% EtOAc. The extractives were qualitatively and quantitatively analyzed in terms of PS and PSMME contents by gas chromatography-flame ionization detector (GC-FID), gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography (HPLC) and proton nuclear magnetic resonance (1H-NMR) spectroscopy. [ABSTRACT FROM AUTHOR]

The lipophilic and hydrophilic extractives in the sapwood (sW) and heartwood (hW) of stems from Pinus halepensis Mill and Eucalyptus camaldulensis Dehnh trees grown in the north of Algeria were analyzed. The extraction of dried samples was carried out in an accelerated solvent extractor (ASE). The lipophilic substances were first extracted with n-hexane and then the hydrophilic ones with acetone/water. The extractives were analyzed by gas chromatography-flame ionization detection (GC-FID), GC-mass spectroscopy (MS) and high-performance size-exclusion chromatography (HPSEC). The largest amount of lipophilic extractives (≈13.4 mg g-1) was observed in the hW of P. halepensis, while the hW of E. camaldulensis contained the largest amount of hydrophilic extractives (≈116.3 mg g-1). Lipophilic extractives are mainly composed of oleoresins (resin acids, terpenes), fats (fatty acids, glycerides, steryl esters, sterols) and waxes (fatty alcohols). Hydrophilic extractives are composed of polyphenols (stilbenes, flavanols), sugars (monosaccharides) and sugar alcohols (cyclic polyols). The main identified lipophilic extractives are resin acids in pine and glycerides in eucalypt. The main identified hydrophilic extractives are cyclic polyols in pine and flavanols and monosaccharides in eucalypt. The total content of extractives is higher in hW than in sW. [ABSTRACT FROM AUTHOR]

Hemicellulose O-acetyl-galactoglucomannan (GGM) is the main noncellulosic water-soluble polysaccharide in the coniferous softwood Norway spruce, consisting of anhydro-galactose, -glucose, and -mannose. Acid hydrolysis of GGM has been studied in a continuous tube reactor to obtain these sugars under industrially relevant conditions. The reaction was performed under atmospheric pressure at 90°C and 95°C, and hydrochloric acid (HCl) served as catalyst. The influence of the reaction parameters, such as acid concentration (pH), temperature, concentration of the substrate, as well as catalyst and reactant flow rates, has been studied on the conversion efficiency and product distribution. Continuous production of monomeric sugars was achieved without formation of low-molecular by-products. The GGM conversion was high with HCl as catalyst, at 95°C, and a pH of 0.3. The main hydrolysis products were mannose, glucose, and galactose monomers. Minor amounts of sugar dimers were detected among the products. The experimental results are described with a laminar flow model for the continuous reactor. [ABSTRACT FROM AUTHOR]

Various lignin determination methods have been applied to hemicellulose-rich wood extracts obtained after pressurized hot-water extraction (PHWE) and membrane ultrafiltration (UF). In focus were the chlorine number (Cl no.) method, the acetyl bromide method, and the four modifications of the Klason lignin determination, such as the KCL, TAPPI, LAP, and Goldschmid methods. The furfural (F) and hydroxymethylfurfural (HMF) concentrations in the acid hydrolysates were also determined. The mass balances of the fraction were calculated with respect to the contents of dry solids and lignin, including the acid-soluble lignin. The reliability of the methods was evaluated based on the lignin mass balances and the gross chemical composition of the extracts. Although the results were dependent on the method applied, the lignin mass balance calculations yielded similar results in general. [ABSTRACT FROM AUTHOR]

The extraction conditions have been evaluated concerning the recovery of specific polyphenols from Scots pine (Pinus sylvestris) knots by means of an accelerated solvent extractor. The composition of the extracts was determined by gas chromatography, gas chromatographymass spectrometry, and high-performance size-exclusion chromatography. The main phenolic compounds are the stilbenes pinosylvin and its monomethyl ether and the lignan nortrachelogenin (NTG), and their amounts vary a lot from sample to sample. The sequential extraction with a nonpolar solvent as a first step for removing the lipophilic compounds was the most efficient approach for the recovery of both pinosylvins and NTG. For food applications, hot water and 85% aqueous ethanol were good solvents for the production of the substances in focus. An industrial knotwood sample from a pulp mill was sequentially extracted with cyclohexane and ethanol/water (95:5) in a large-scale Soxhlet equipment. The results show that the industrial production of pinosylvins and NTG from knots is feasible. [ABSTRACT FROM AUTHOR]