Method for silver fir wood green

FIELD: food industry.

SUBSTANCE: method for processing silver fir wood green envisages raw material milling, the raw material treatment with an alkali solution, the raw material filtering to remove the resultant solution, acids separation by way of extraction with an organic solvent. After milling the raw material is treated with 0.1-0.5% water solution of a mineral acid at a temperature of 50±5°C with the filtered raw material subsequent two-times washing with water. Then the blended acid filtrates are concentrated by way of water boiling out in a rotor evaporator at a temperature of 60°C. Polysaccharides are sedimented from the resultant concentrate with excessive ethanol. The raw material remaining after polysaccharides extraction is subjected to treatment with an alkali and an organic solvent to separate triterpenic acids.

EFFECT: invention enables silver fir wood green processing to produce polysaccharides and triterpenic acids and to increase the target products yield.

2 ex

 

The invention relates to the field of processing of vegetable raw materials, namely wood green fir the purpose of separation from her pectic polysaccharides and triterpene acids. The invention can be used in pharmaceutical. the medical industry, in agriculture.

There is a method of processing wood green fir [patent SU 1375226]. includes grinding of raw materials and the extraction of essential oils by distillation with steam to obtain a solid residue, followed by treatment with a solution of isopropyl alcohol, insisting at 30-60°C with further filtering, cooling, defending it until it separates into 2 layers and evaporation of each layer separately. From the upper layer to obtain natural pine extract, the bottom layer is used for chlorophylla-carotene paste. From the remainder of the wood green prepare vitamin flour. This method does not allow to allocate in the form of product pectin.

There is a method of processing wood green pine [patent RU 2364409], including chopping wood greenery and extraction, defending the obtained extract, Department of wax raw, stripped of solvent and essential oils, saponification one stripped off of the extract with alkali. The extraction of raw materials spend gasoline or hexane extraction residue is carried out in two stages: the first 80-90%aqueous solution of ethyl alcohol at a temperature of 80-85°C with separation of the extract and cake the second hydrolysis-extraction meal exercise equimolar mixture of 0.5%ammonium oxalate solution and 0.5%oxalic acid at a temperature of 60-80°C, followed by separation of pectin substances from ethanol. The invention allows to obtain pectin pine as a separate product.

There is a method of isolating biologically active amount of the acid from the wood green fir [patent RU 2161149]. taken as a prototype. The method consists in grinding raw materials, processing of raw materials with an aqueous solution of alkali, filtering of the raw material from the resulting solution, the allocation of the triterpene acids from the solution by extraction with an organic solvent after the destruction of the salts of the acids. The known method does not allow efficient enough to process the green wood fir the purpose of obtaining the range of available products.

The technical result consists in extending the functionality of the method of processing wood green of fir and expansion of products of processing of raw materials, pectic polysaccharides and acids.

The technical result is achieved in that the method of processing wood green fir includes the grinding of raw materials, processing of raw materials with an aqueous solution of alkali, filtering of the raw material from the resulting solution, the selection of acids by extraction with an organic solvent, according to from the retenu after grinding the raw material is treated with 0.1-0.5%aqueous solution of mineral acid at a temperature of 50±5°C, followed by washing twice with water filtered raw materials, the concentration of the combined acidic filtrate by evaporation of the water on a rotary evaporator at 60°C and precipitation of polysaccharides from concentrate an excess of ethyl alcohol, and treatment with alkali and subjected to solvent remaining after the extraction of polysaccharides raw materials.

The task is solved as follows.

The method of processing wood green fir based on the processing of the crushed material is 0.1-0.5%aqueous solution of mineral acid at a temperature of 50±5°C, subsequent double the washing water filtered raw materials, deposition of polysaccharides from the United acidic filtrates excess of ethyl alcohol, the processing of raw materials an aqueous-alkaline solution, separating by filtration the resulting aqueous-alkaline solutions, acids extraction with an organic solvent after acidification of the aqueous-alkaline solution.

Example 1. Preliminary grinding of raw materials was performed on a disk grinder to a fraction of 80-100 mm, Then the grinding was performed on screw grinder to a fraction of 1.0-3.0 mm

The reactor was filled powdered raw materials in the amount of 1 kg, then filled in 10 l of 0.5%aqueous hydrochloric acid solution temperature of 50°C. the process water ratio 1/10. Processing was carried out for 2 hours. After processing, the mixture was filtered, then the green wood with filter is arenosillo in the reactor, was filled with 5 l of water (water ratio 1/5) 50-55°C and washed under stirring for 30 minutes the mixture is Then filtered, transferred into the reactor and washed raw water for the second time.

The combined acidic filtrate was concentrated by evaporation of water on a rotary evaporator at 60°C to a volume of 2.4 liters

From concentrate polysaccharides were planted threefold excess of 96%ethyl alcohol. Polysaccharides were filtered on a Buechner funnel, washed three times with ethanol, dried in the air. Polysaccharide yield was 3% by weight of the feedstock.

Processing remaining after extraction of the polysaccharides of the raw materials was performed using a 5%aqueous sodium hydroxide solution (water ratio 1/10) at 50-55°C for 2 hours. The resulting aqueous-alkaline solution was filtered from recycled raw materials.

The obtained alkaline filtrate was acidified using 20%aqueous sulfuric acid solution to pH=3 and extracted with diethyl ether. The extract obtained was washed with water until neutral, dried anhydrous Na2SO4that was evaporated on a rotary evaporator. Received the extract triterpenoic acids with the release of 5.6% by weight of the feedstock.

Example 2. The raw materials are carried out analogously to example 1. except for the concentration of hydrochloric acid, which amounted to 0.1%. You are the od of the polysaccharides was 2.6% by weight of the feedstock.

The method of processing wood green fir, including the grinding of raw materials, processing of raw materials with an aqueous solution of alkali, filtering of the raw material from the resulting solution, the selection of acids by extraction with an organic solvent, characterized in that after grinding the raw material is treated with 0.1 to 0.5%aqueous solution of mineral acid at a temperature of (50±5)°C, followed by washing twice with water filtered raw materials, the concentration of the combined acidic filtrate by evaporation of the water on a rotary evaporator at 60°C and precipitation of polysaccharides from concentrate an excess of ethyl alcohol, and treatment with alkali and subjected to solvent remaining after the extraction of polysaccharides raw materials.



 

Same patents:

FIELD: food industry.

SUBSTANCE: invention relates to technical biochemistry, in particular - to determination of pectin substances quantity in vegetal raw material. "Standardised" solutions of pectin substances fractions are prepared. The fractions solutions are sampled. Saponification of pectin substances fractions in the samples of the solutions being analysed is performed with 2.5 ml of 40% NaOH solution. The pectin substances fractions are sedimented with 2.5 ml of concentrated HCl. The solutions being analysed are centrifuged in 50 ml test tubes, rotation frequency being no less than 500 rpm, during 5-7 minutes. The sediments of pectin substances fractions are suspended in distilled water in a titration cup on a magnetic stirrer for at least 30 minutes. One performs conductometric titration of the suspension of pectin substances fractions sediment, stirring. Following the conductometric titration results, graphs are drawn, relying whereon one identifies the volume of the titrant spent on pectin acid titration. Pectin substances fractions weight percentage is calculated from the formula: ω=176×0,2×V10×200×100, where 176 - pectin acid equivalent; 0.2 - titrant normality; V - titrant volume spent on pectin acid titration, ml; 200 - volume of the solution of the corresponding pectin substances fraction taken for analysis, ml; 10 - conversion to acid milliequivalents (1 ml of 0.1n NaOH corresponding to 0.1 acid milliequivalent); 100 - percentage conversion factor.

EFFECT: invention enables obtainment of accurate data with high coincidence of parallel analyses and ensures labour and time expenditures saving at all the process stages.

6 dwg, 1 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to methods for preparing low-molecular pectin and may be used in pharmaceutical industry for preparing new therapeutic and preventive drugs, low-molecular sorbents. The method provides pectin hydrolysis in an aqueous solution of mineral acid and liquid phase separation from an insoluble residue of pectin. The low-molecular products of pectin hydrolysis are recovered from the liquid phase by settling them in an organic solvent with water. A hydrolysis feed material is low-etherified pectin of ratio max. 30%. The hydrolysis process is continuous in a continuous-flow machine. Temperature in a working chamber of the machine is maintained at 70-100°C. Feeding speed of mineral acid into the chamber is calculated by specific formula. The prepared liquid phase is neutralized to pH min. 4.0. Thereafter, the prepared liquid phase is used to settle the low-molecular products of pectin hydrolysis.

EFFECT: invention enables producing low-molecular pectin with no process loss of the feed material, substantially reducing oligogalacturonide destruction accompanying the hydrolysis process, and thereby improving the end product yield.

5 cl, 1 dwg, 4 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to methods for preparing low-molecular pectin and may be used in pharmaceutical industry for preparing new therapeutic and preventive drugs, low-molecular sorbents. The method provides pectin hydrolysis in an aqueous solution of mineral acid with heating and liquid phase separation from an insoluble residue of pectin. The low-molecular products of pectin hydrolysis are recovered from the liquid phase by settling them in an organic solvent with water. A hydrolysis feed material is low-etherified pectin of ratio max. 30%. The hydrolysis process is continuous in a continuous-flow machine. Temperature in a working chamber of the machine is maintained at 70-100°C. Feeding speed of mineral acid into the chamber is calculated by specific formula. The prepared liquid phase is exposed to additional heat treatment in a flow heat exchange following the hydrolysis process. Temperature of the additional heat treatment process coincides with hydrolysis temperature. Heat exchange section capacity is determined by specific formula. The prepared liquid phase is neutralised to pH min. 4.0. Thereafter, the prepared liquid phase is used to settle the low-molecular products of pectin hydrolysis.

EFFECT: invention enables producing low-molecular pectin with no process loss of the feed material, substantially reducing oligogalacturonide destruction accompanying the hydrolysis process, and thereby improving the end product yield.

5 cl, 1 dwg, 4 ex

FIELD: food industry.

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3 ex

FIELD: food industry.

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EFFECT: invention allows to produce pectin polysaccharides and glucuron- oxylan class hemicellulases of coniferous trees greens with high yield and high purification degree.

7 cl, 1 dwg, 1 tbl, 4 ex

FIELD: chemistry.

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EFFECT: invention enables to obtain low-molecular pectin without process loss of material and also significantly ensures destruction of oligogalacturonides, thus increasing ultimate output of the product.

2 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing low-molecular pectin. The method involves hydrolysis of pectin in aqueous solution of mineral acid while heating. Further, the liquid phase is separated from the insoluble pectin residue and neutralised to pH lower than 4.0. Low-molecular pectin hydrolysis products are extracted through precipitation thereof using a water-miscible organic solvent. After precipitation, the obtained low-molecular pectin hydrolysis products are dried. The starting material used for hydrolysis is low-etherified pectin with etherification degree of not more than 30%. Hydrolysis is carried out in cycles. The duration of one cycle is calculated using a given formula. After separation from the pectin residue, the liquid phase undergoes further hydrolysis. The duration of one cycle of additional hydrolysis is calculated using a formula.

EFFECT: invention enables to obtain low-molecular pectin without process loss of material and also significantly ensures destruction of oligogalacturonides, thus increasing ultimate output of the product.

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FIELD: chemistry.

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4 cl, 2 dwg, 1 tbl, 6 ex

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2 tbl, 1 ex

FIELD: medicine.

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EFFECT: improved isolating method.

FIELD: vegetable raw technology.

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EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw. Method for preparing pectin from citrus husks involves hydrolysis-extraction of a solid phase and separation of a liquid phase. Before hydrolysis-extraction a solid phase is extracted with dimethylformamide and liquid acetylene successively under the above atmosphere pressure. The second extract is separated without pressure change followed by abrupt dropping pressure over a solid phase up to atmosphere value and feeding a solid phase to hydrolysis-extraction. Invention provides reducing loss of pectin being without deterioration of its organoleptic properties.

EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw. Method for isolating pectin from citrus husks involves hydrolysis-extraction of a solid phase and separation of a liquid phase. Before hydrolysis-extraction a solid phase is extracted with dimethylformamide and liquid carbon dioxide successively under the above atmosphere pressure. The second extract is separated without the pressure change followed by abrupt dropping pressure over a solid phase up to atmosphere value and feeding a solid phase to hydrolysis-extraction. Invention provides reducing loss of pectin being without deterioration of its organoleptic properties.

EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw. Method for preparing pectin from citrus husks involves hydrolysis-extraction of a solid phase and separation of a liquid phase. Before hydrolysis-extraction a solid phase is extracted with acetone and liquid carbon dioxide successively under the above atmosphere pressure. The second extract is separated without pressure change followed by abrupt dropping pressure over a solid phase up to atmosphere value and feeding a solid phase to hydrolysis-extraction. Invention provides reducing loss of pectin being without deterioration of its organoleptic properties.

EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for preparing pectin extract from vegetable raw. Method involves the successive extraction of citrus husks with acetone. Then after separation of extract a solid phase is extracted with a mixture of liquid acetylene and carbon dioxide taken in mass ratio from 3:7 to 7:3. Then hydrolysis-extraction of a solid phase is carried out and a liquid phase is separated after termination of the hydrolysis-extraction process. Method provides reducing loss of pectin.

EFFECT: improved isolating method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw. Method for preparing pectin involves milling and mixing sunflower heads and citrus husks, hydrolysis-extraction of mixture, separation of a liquid phase and isolation of the end product from its. Before mixing sunflower heads and citrus husks are extracted with ethyl acetate and liquid carbon dioxide separately and successively under the above atmosphere pressure. The second extract is separated without pressure change followed by dropping pressure over a solid phase up to atmosphere value and feeding a solid phase to hydrolysis-extraction. Invention provides enhancing quality of the end product due to elimination of undesirable taste and odor and without deterioration of its technological properties and without reducing the specific yield of pectin.

EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw. Method for preparing pectin involves milling and mixing sunflower heads and citrus husks, hydrolysis-extraction of mixture, separation of a liquid phase and isolation of the end product from its. Before mixing sunflower heads and citrus husks are extracted with acetone and liquid carbon dioxide separately and successively under the above atmosphere pressure. The second extract is separated without pressure change followed by abrupt dropping pressure over a solid phase to atmosphere value and feeding a solid phase to hydrolysis-extraction. Invention provides enhancing quality of the end product due to elimination of undesirable taste and odor and without deterioration of its technological properties and without reducing the specific yield of pectin.

EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for preparing pectin from vegetable raw. Method for preparing pectin involves milling and mixing sunflower heads and citrus husks, hydrolysis-extraction of mixture, separation of a liquid phase and isolation of the end product from its. Sunflower heads and citrus husks are extracted with dimethylformamide and liquid carbon dioxide before mixing separately and successively and corresponding extracts are separated. After separation of the second extract pressure is dropped abruptly up to atmosphere value, solid phases of sunflower heads and citrus husks are mixed and fed to hydrolysis-extraction. Invention provides enhancing quality of the end product due to elimination of undesirable taste and odor being without deterioration of its technological properties and without reducing the specific yield of pectin.

EFFECT: improved preparing method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for preparing pectin from vegetable raw. Method for preparing pectin involves milling and mixing sunflower heads and citrus husks, hydrolysis-extraction of mixture, separation of a liquid phase and isolation of the end product from its. Citrus husks and sunflower heads are extracted acetone and liquid acetylene before mixing separately and successively at the above atmosphere pressure. The second extract is separated without pressure change followed by abrupt dropping pressure up to atmosphere value and a solid phase is fed to hydrolysis-extraction after mixing. Invention provides enhancing quality of the end product due to elimination of undesirable taste and odor being without deterioration of its technological properties and without reducing the specific yield of pectin.

EFFECT: improved preparing method.

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