Xylan extraction yields

The most common method to extract xylan is the alkaline extraction. Several pretreatment methods can be used in association in order to break the covalent bonds that exist between xylan and other carbohydrates during the extraction (Wang Zhang, 2006). A number of articles studied the use of ultrasound on the xylan extraction. Hromadkova and coworkers reported that 36.1% of xylan was extracted from corn cobs with 5% NaOH solution at 60°C for 10 min of ultrasonication in comparison with 31.5% of xylan in the classical extraction. Both extractive methods yielded xylan with immunogenic properties (Hromadkova et al., 1999). 

The efficiency of extraction was observed to be inversely proportional to the corn cob particle size. This was expected because the size reduction corresponds to an increase in total particle surface area. An increase in the time of the alkaline extraction and in the NaOH concentration also improves the efficiency of xylan extraction. This happened because when the NaOH concentration was lower, the xylan present in corn cobs could not be fully dissolved in the solution. Thus, it resulted in lower efficiency of xylan extraction. However, when the NaOH concentration was higher than 2 M, the yields decreased with continuously increasing of the NaOH concentration. This is probably due to the alkaline degradation of xylan chains, proceeding at the higher NaOH concentration, which indicated that the ideal NaOH concentration in the extraction was between 1.5 and 1.8 M (Unpublished data). 

In an attempt to isolate a water-soluble 0-acetyl-(4-0-methylglucurono)-xylan from a birch chlorite holocellulose, Marchessault and coworkers kept the time of contact between the ammonia and the holocellulose at a minimum. Successive extractions of the pretreated holocellulose with water and methyl sulfoxide removed the xylan in yields of 7.1 and 14.6%, respectively, based on the weight of the original wood. The products still contained most of the iironic acid, but only one third of the 0-acetyl groups of the native xylan. 

The best results for both the extraction yield in the hemicellulosic powder and the sugar purity in the case of xylan extraction from wheat bran in a twin-screw extmder are obtained for a low NaOH ratio (bran/soda = 7) and a low straw content. 

The total alkaline charge required for xylan extraction was of major importance for the feasibility of the isolation process. These factors were dependant on the alkalinity of the extraction liquor and the consistency used in the process. In Figure 1 the effect of alkalinity on the yield of xylan and extraction residue is depicted for 10% and 25% consistency. The upper picture for 10% consistency demonstrates that an increase of NaOH concentration from 2.2 to 5% resulted in a continuous increase of xylan yield. Totalling the yield of xylan and residue it became apparent that up to 20% of the starting materials were not recovered. This material remained in the precipitation liquid and should consist of extractives, lignin fragmentation products, and low molar mass carbohydrates. A further analysis of those components was not pursued at this stage of the project. 

Non-pressurized and O2 aided extraction were further compared at 90 °C and 10% consistency, performing the extraction ei t times for each condition. The results in Table IV demonstrate that a high reproducibility of 0.3-0.4% could be achieved regarding the extraction yield. The non-pressurized extraction had a 1.4% higher yield of xylan powder compared to the 02-aided procedure. However, this difference resulted from a higher lignin content as indicated by... 

A xylan extracted from the holocellulose present in the stalks of Nicotiana tabacum has been purified by ion-exchange chromatography. The results of methylation analysis, partial hydrolysis with acid, and enzymic hydrolysis indicated that the xylan is composed of a straight chain of approximately 100 /S-(l -> 4)-linked D-xylopyranosyl residues. Curie point-g.l.c. of the xylan yielded 2-furaldehyde, which is probably formed via 3-deoxy-D- /ycero-pent-2-ulose. Another major product was identified as 3-hydroxy-2-penteno-1,5-lactone (21) by high-resolution m.s. this lactone has also been prepared by pyrolysis of a hexuronic acid-containing xylan from beech. Since the tobacco-stalk xylan contains no acidic components, the lactone (21) must arise by... 

Thermoplastic xylan derivatives have been prepared by in-hne modification with propylene oxide of the xylan present in the alkaline extract of barley husks [424,425]. Following peracetylation of the hydroxypropylated xylan in formamide solution yielded the water-insoluble acetoxypropyl xylan. The thermal properties of the derivative quahfy this material as a potential biodegradable and thermoplastic additive to melt-processed plastics. Xylan from oat spelts was oxidized to 2,3-dicarboxyhc derivatives in a two-step procedure using HI04/NaC102 as oxidants [426]. 

Hemicelluloses are quite difficult to extract from cell walls of softwoods (9,10) and are usually destroyed or depolymerized during the chemical pulping of these raw materials. However, other hemicelluloses, primarily xylans, can be extracted by cold, dilute sodium hydroxide from grasses and many hardwoods in very high yields (9,77). These xylans are deacetylated in an alkaline medium and are for the most part insoluble (hemicellulose A). A partially water soluble fraction (hemicellulose B) has also been... 

The particular wood species we chose for this study is aspen (Populus tremuloides), which is plentiful in Canada and in the northern U.S.A. The chemical composition we found to be glucan 53.4%, xylan 14.9%, total carbohydrate 79.0%, lignin 17.1% and extractives 3.8%. We would expect total fermentable sugars of about 56% in this sample of aspen in anhydro form (Timell has reported about 60% in another sample (15)) which upon hydrolysis would yield about 1,250 lb wood sugars per ton of wood (dry basis), from the stoichiometry. Theoretical conversion of this sugar to ethanol would yield 640 lb or 81.1 gallons of anhydrous... 

That not all of the xylans of wood are homogeneous polymers of anhydro-D-xylose units has been shown by the classical studies of O Dwyer (1923 to 1940) on hemicelluloses of American white oak. O Dwyer prepared a hemi-cellulose fraction from water-extracted, oakwood sawdust by extraction for two days with 4% aqueous sodium hydroxide solution. The polysaccharide material was obtained, after acidification, by the addition of ethanol. The product ([a]n —75° in 1 % sodium hydroxide), contained 70% of pentosan, and yielded n-xylose, n-maiinose, n-galactose, and L-arabinose on hydrolysis. 

For isolation of hardwood xylans by way of holocellulose, a choice has to be made between the different methods available, according to the objectives to be attained. If molecular properties are to be investigated, the modified chlorine-2-aminoethanol method and, possibly, also the method of Klauditz are suitable. For chemical studies, especially if the location of the 0-acetyl groups is to be established, only chlorine dioxide or chlorous acid can be used. The subsequent extraction of the holocellulose will also have to be adapted to the desired ends. For isolation of a pure (4-0-methylglucurono)xylan, aqueous potassium hydroxide is excellent, since it gives almost quantitative yields and seldom causes removal of the gluco-mannan. If necessary, further purification can be effected by precipitation with Fehling solution. - ... 

In an attempt to improve the yield of hemicelluloses. Sands and Nutter subjected mesquite (Prosopis julifiora) wood to alternate extraction with alkali and delignification with chlorine and aqueous ammonia. The resulting fractions all consisted of a xylan whose average composition corresponded to one methoxyl group, one uronic acid residue, and ten xylose residues, or exactly the same composition as had been noted by O Dwyer for her oak xylan." ... 

Bird and Ritter isolated, from wood of white oak, a chlorine holocellu-lose which contained all of the 0-acetyl groups present in the wood. Mitchell and Ritter later extracted a chlorine holocellulose from sugar maple with water and obtained a xylan in a yield of 3.4% of the wood. This polysaccharide contained 9.2% of 0-acetyl groups. A xylan which had been obtained in the same way, from aspen, by Wise and Jones, was, on treatment with periodate, oxidized almost to completion. When the wood itself was similarly treated, most of its xylan escaped oxidation. Although it appears evident that all of the xylan in the wood could not possibly have been accessible to the aqueous reagent, it was concluded that the lack of oxidation was most probably due to the fact that the native xylan was partly 0-acetylated. After treatment of wood from Eucalyptus regnans with methanol at 150°, Stewart and coworkers obtained, on extraction with water, a xylan (in a jdeld of 3.7%) which contained 5-6% of acetate... 

A chlorite holocellulose from white-birch wood, on extraction with methyl sulfoxide, gave a xylan containing 5.3 0-acetyl groups per ten xylose residues. In this case, the yield was only 5% of the original wood. The hemi-cellulose contained 58.1% of unsubstituted, 11.8% of 2-0-substituted, 24.0% of 3-0-substituted, and 6.1% of 2,3-di-O-substituted xylose residues. The 0-acetyl groups in native hardwood xylans are thus distributed between C-2 and C-3 of the xylose residues, with the majority located at C-3. It should, perhaps, be pointed out that, so far, only this species has been investigated, and moreover, only a minor part (15%) of the xylan portion of this wood has been studied. 

As mentioned previously (see Part I, p. 255), only minor quantities of hemicelluloses can be removed from softwood by direct extraction with alkali. Very likely, the hemicelluloses are protected by the lignin, especially by that portion which surrounds the polysaccharides in the secondary wall. Isolation of softwood xylans by direct, alkaline extraction of tbe wood seems to have been used on only two occasions. Saarnio, using wood shavings of Norway spruce Picea abies), was able to obtain a relatively pure arabino-(4-0-methylglucurono)xylan in a yield of 3%, simply by extracting with 5% aqueous potassium hydroxide, a remarkable result. With wood of loblolly pine, Jones and Painter obtained a mixture of hemicelluloses, in a yield of about 1%, on direct extraction with 25% aqueous potassium hydroxide solution containing 4% of borate. 

Xylan is a wood gum which is found in the bark of trees. It can be obtained by extracting pine-wood sawdust or straw with dilute sodium hydroxide, and precipitating the alkaline solution with alcohol and hydrochloric acid. Xylan is a porous mass which dissolves in hot water to form a solution that becomes opalescent on cooling. It yields xylose when hydrolyzed by acids when distilled with acids, the xylose formed is converted into furfurol. 

Alkaline extraction of the husks of Ispaghula has yielded a highly branched acidic L-arabino-D-xylan. The polysaccharide is unusual in containing both (l->3)- and (14)-D-xylose residues in the main chain with the majority of residues further substituted at 0-2 or 0-3 with residues of L-arabinose, D-xylose, or D-galactopyranosyluronic acid-(l2)-L-rhamnose. Another acidic polysaccharide, based on a (14)-D-xylan main chain has been isolated from the seeds of Ocimum basilicum The polysaccharide contained D-xylose, L-arabinose, L-rhamnose, and D-galacturonic acid in the molar ratio 15 9 7 12 and the branch points were present at both 0-2 and 0-3 of the D-xylose residues in the main chain. Two oligosaccharide sequences, (15) and (16), were isolated from the side chains. 

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