Method for preparing pectin

FIELD: technology of natural substances.

SUBSTANCE: invention relates to a method for isolating pectin from vegetable raw used for production of products of prophylactic and curative designation. Invention describes a method for preparing pectin. Method involves treatment of preliminary milled vegetable raw, for example, dried sunflower heads with a mixture of chloroform and ethanol followed by extraction in water bath at 70-80°C for 30-40 min, filtration and separation of the first extract. Filtered off vegetable raw is poured with distilled water at temperature 60-70°C and extracted in water bath at temperature 90-95°C for 1 h followed by filtration and separation of the second extract. Filtered off vegetable raw is poured with 0.3-0.5% ammonium oxalate solution, extracted in water bath at temperature 75-80°C for 30-40 min, filtered and the third extract is separated. Filtered off vegetable raw is poured with a 0.4-0.5% hydrochloric acid solution, heated at temperature 75-80°C for 1 h followed by filtration and separation of the fourth extract that is mixed with prepared first, second and third extracts. Prepared solution is neutralized with ammonium hydroxide to pH 7 and precipitated with 96% ethyl alcohol, precipitate is squeezed our and dried at temperature 4-6°C. Proposed method provides increasing yield of pectin and its solubility.

EFFECT: improved preparing method.

2 cl, 1 ex

 

The invention relates to the process of extracting pectin from plant materials, namely, to a method for gelling of the product, and can be used in the manufacture of products of mass consumption prophylactic and therapeutic purposes.

A known method of producing pectin from vegetative organs of plants violets, in which air-dry raw material (moisture content of 8.4-9.0 per cent) was sequentially treated with chloroform and methanol to remove colored substances and low molecular weight products. Carbohydrates were isolated by well-known methods of fractional extraction. Extraction of water-soluble polysaccharides (VRPS) was performed with hot water at 90-95° (1:20) 2 hours an Aqueous extract was filtered, evaporated and treated with 96%ethanol. The precipitate was separated by centrifugation, washed with ethanol, acetone and dried under vacuum for 6 hours. The output of 8.5-12.3 per cent. (Sabana H. Polysaccharides Viola tricolor // Chemistry of natural compounds, 1985, No. 1. - C.116).

The disadvantage of this method is the use of methanol - toxic substances that require special conditions of storage and evaporation of solutions of pectin, which leads to partial dimethoxypropane and poor solubility of the drug, as well as the insufficient output of pectin.

The technical result consists in increasing the yield of pectin and improve its solubility.

Technical is such a result is achieved by the method of producing pectin which consists in the fact that pre-shredded plant material is treated with a solution of chloroform and ethanol, prepared in a ratio of 1:3, taken respectively in the ratio of 1:6 with subsequent extraction in a water bath at a temperature of 75-80°C for 30-40 minutes, followed by filtration plant materials for separating the first extract. Filtered vegetable raw material is poured into distilled water at a temperature of 60-70°respectively in the ratio of 1:18 and extracted in a water bath at a temperature of 90-95°C for one hour followed by filtration plant materials for separating the second extract. Filtered vegetable raw material is poured 0,3-0,5% solution of ammonium oxalate, respectively, in the ratio of 1:15 and extracted in a water bath at a temperature of 75-80°C for 30-40 minutes, followed by filtration plant materials for the Department of the third extract. Filtered vegetable raw material is poured 0,4-0,5% solution of hydrochloric acid and extracted at a temperature of 75-80°C for one hour followed by filtration plant materials for the Department of the fourth extract, which is mixed with the received first, second and third extracts, the resulting solution is neutralized with hydroxide is ammonia to pH 7, precipitated with 96% ethanol, respectively, in the ratio of 1:3 at room temperature. Received the precipitation is squeezed and dried at a temperature of 4-6°C. as plant materials used basket dried sunflower.

The concentration of ammonium oxalate 0.3 to 0.5% corresponds to conduct extraction, less than 0.3% reduces the yield of pectin concentration of ammonium oxalate than 0.5% disrupts the molecular structure of pectin. The extraction of vegetable raw materials should be carried out at a temperature of 75-80°C for 30-40 minutes in order to avoid thermal degradation of pectin macromolecules.

When the extraction of the raw material solution of hydrochloric acid with a concentration of 0.3-0.5% at a temperature of 75-80°C for 1 hour created optimal conditions to increase the yield of pectin without damaging its structure. The concentration of hydrochloric acid more than 0.5%, increasing the duration of extracting more than 1 hour can reduce the content metaxylene groups in the pectin macromolecule, which negatively affects the quality of pectin.

The precipitation of pectin is dried at a temperature of 4-6°With, at the same temperature are stored gelling properties of pectin, not prone to splitting and improves its solubility.

The method is as follows.

Prepare the extras the Gent (solution) of chloroform and ethanol in the ratio 1:3. Basket dried sunflower crushed and receive plant material, which is then poured prepared by the extractant, with a ratio of 1:6 and extracted in a water bath at a temperature of 75-80°C for 30-40 minutes to remove the dye and resinous substances, then filtered. The first extract is poured into a separate container. Filtered vegetable raw material is poured into distilled water at a temperature of 60-70°With the ratio of 1:18 and extracted in a water bath at a temperature of 90-95°C for 1 hour. Plant material is filtered off, get a second extract. Filtered vegetable raw material is poured 0,3-0,5% solution of ammonium oxalate in the ratio of 1:15 and extracted in a water bath at a temperature of 75-80°C for 30-40 minutes. Plant material is filtered off, get the third extract. Then filtered vegetable raw material is poured 0,4-0,5% solution of hydrochloric acid and extracted at a temperature of 75-80°C for 1 hour. Plant material is filtered to separate the fourth extract. All obtained extracts are mixed and neutralized with ammonium hydroxide to pH 7. The pectin from the combined extracts precipitated with 96% ethanol in the ratio 1:3 at room temperature. The precipitate pectin sucked, squeezed through the hygroscopic material and high who're asked at a temperature of 4-6° C

Compared with the known solution the proposed method allows to increase the intensity of the extraction process and the selection of the optimal number precipitator, which ensures maximum efficiency of extraction and precipitation of pectin from medicinal raw materials. Baskets sunflower seeds contain significant amounts of pectin, so you can use them as a promising raw material source for the production of this class of biologically active substances.

1. The method of producing pectin which consists in the fact that pre-shredded plant material is treated with a solution of chloroform and ethanol, prepared in a ratio of 1:3, taken respectively in the ratio of 1:6 with subsequent extraction in a water bath at a temperature of 75-80°C for 30-40 min, followed by filtration plant materials for separating the first extract, filtered vegetable raw material is poured into distilled water at a temperature of 60-70°respectively in the ratio of 1:18 and extracted in a water bath at a temperature of 90-95°C for one hour, followed filtration plant materials for separating the second extract, filtered vegetable raw material is poured 0,3-0,5%solution of oxalic acid ammonium, respectively, in the ratio of 1:15 and extracted in a water bath is when the temperature of 75-80° C for 30-40 min, followed by filtration plant materials for the Department of the third extract, filtered vegetable raw material is poured 0,4-0,5%solution of hydrochloric acid and heated at a temperature of 75-80°C for one hour followed by filtration plant materials for the Department of the fourth extract, which is mixed with the received first, second and third extracts, the resulting solution is neutralized with ammonium hydroxide to pH 7, precipitated with 96% ethanol, respectively, in the ratio of 1:3 at room temperature, the obtained precipitated sludge is squeezed and dried at a temperature of 4-6°C.

2. The method of producing pectin according to claim 1, characterized in that as the plant materials used basket dried sunflower.



 

Same patents:

FIELD: pectin production.

SUBSTANCE: dry pectin extract is subjected to six-step extraction with aqueous ethanol solution under the next process parameters: 1) 35-40 % solution, pH 2-2.5; temperature of 45-50°C, and solid/liquid phase ratio of 1:(1-1.5); 2) 45-50 % solution, pH 2.5-2.8; temperature of 50-55°C, and solid/liquid phase ratio of 1:(1.5-2); 3) 55-60 % solution, pH 2.8-3, temperature of 40-50°C, and solid/liquid phase ratio of 1:(2.5-3); 4) 65-75 % solution, pH 3-3.2; temperature of 50-55°C, and solid/liquid phase ratio of 1:(2-2.5); 5) 75-80 % solution, pH 3.2-3.5; temperature of 45-50°C, and solid/liquid phase ratio of 1:(2-2.5); 6) 80-85 % solution, pH 3.2-3.5; temperature of 30-40°C, and solid/liquid phase ratio of 1:(1-2.5). Isolated solid phase is further dried.

EFFECT: pectin of increased complexing ability.

FIELD: pectin production.

SUBSTANCE: claimed method includes swelling of plant raw materials, hydrolysis, and extraction by using of polyharmonic vibration of 15-50 Hz frequency, wherein swelling and hydrolysis are carried out in one step with hydrochloric acid solution followed by separation of solid and liquid phases and recycling of the last in swelling and hydrolysis step. Separated solid phase is diluted with water and used for extraction of pectin substances under vibration action. Further obtained extract is concentrated and purified in ultrafiltration apparatus to obtain pectin concentrate followed by dying thereof in vacuum drier.

EFFECT: accelerated method for pectin production; reduced reagent consumption.

2 ex, 2 tbl

FIELD: organic chemistry, medicine, pharmacy.

SUBSTANCE: invention describes a water-soluble sodium-, calcium-, iron-polygalactouronate of the general formula (I): used as a stimulating agent of the hemopoiesis process. The compound is prepared by treatment of pectin with alkali NaOH solution at temperature 50-60°C and successive addition of aqueous solution of calcium and iron salts followed by precipitation with alcohol, centrifugation and drying. The compound can be used in using both a solid substance and as solutions for pharmaceutical aims.

EFFECT: valuable medicinal properties of agent.

3 cl, 2 tbl, 4 ex

FIELD: food processing industry, in particular pectin production for beverage manufacturing.

SUBSTANCE: to increase of pectin solubility dry pectin extract is treated by three-step extraction with ethanol aqueous solution under the next conditions: 1) 45-55 % solution, pH 1.5-2, temperature of 45-50°C, and solid/liquid phase ratio of 1:(1-1.5); 2) 45-50 % solution, pH 2-2.5, temperature of 45-50°C, and solid/liquid phase ratio of 1:(1.5-3); 3) 65-70 % solution, pH 6.5-9, temperature of 45-50°C, and solid/liquid phase ratio of 1:(2.5-3); Then solid phase is dried. Obtained pectin has water solubility of 5 % and molecular weight of 40000-50000.

EFFECT: improved method of pure pectin production.

FIELD: food processing industry, in particular pectin production for beverage manufacturing.

SUBSTANCE: to increase of pectin gel-forming ability dry pectin extract is treated by four-step extraction with ethanol aqueous solution under the next conditions: 1) 45-55 % solution, pH 2.5-3, temperature of 50-55°C, and solid/liquid phase ratio of 1:(1-1.5); 2) 60-65 % solution, pH 3-3.5, temperature of 60-65°C, and solid/liquid phase ratio of 1:(1.5-2.5); 3) 65-68 % solution, pH 3.5-3.8, temperature of 55-60°C, and solid/liquid phase ratio of 1:(2.5-3); 4) 65-75 % solution, pH 2.8-3.2, temperature of 50-55°C, and solid/liquid phase ratio of 1:1. Then solid phase is dried.

EFFECT: improved method of pure pectin production.

FIELD: food processing industry.

SUBSTANCE: invention discloses a pectin production process characterized by that starting material utilized is dry coffee purification waste, which is washed with water at 70-80°C for about 1 h and then subjected to hydrolysis and extraction using hydrolysis agent with pH 1.5-3, whereupon liquid phase is separated and target product is recovered therefrom.

EFFECT: enlarged resource of raw materials for production of pectin.

FIELD: food processing industry.

SUBSTANCE: invention discloses a pectin production process characterized by that starting material utilized is wet coffee purification waste, which is washed with water at 70-80°C for about 1 h and then subjected to hydrolysis and extraction at 60-90°C for 1-2 h using hydrolysis agent with pH 1.5-3, whereupon liquid phase is separated and target product is recovered therefrom.

EFFECT: enabled utilization of waste for production of product meeting requirements of corresponding state norm.

FIELD: biotechnological processes.

SUBSTANCE: method of producing pectin from vegetable raw material comprises: (i) first extraction step consisting in contacting vegetable raw material with low-acidic solution having pH not higher than 4.0 and not lower than 2.5 at upper-limit temperature 90°C and lower-limit temperature above 70°C over a period of time long enough to remove calcium-insensitive pectin; (ii) separating extraction liquid from vegetable raw material; (iii) passing separated extraction liquid to heat-exchanger; (iv) removing water from extraction liquid in evaporator; (v) precipitating calcium-insensitive pectin; and (vi) drying and breakage. Alternative embodiment of the method comprises: (i) extracting calcium-insensitive pectin fraction from material and separating extraction liquid; (i) treating remaining vegetable raw material with high-acidic solution having pH not higher than 2.2 and not lower than 1.6 at upper-limit temperature 90°C and lower-limit temperature above 70°C over a period of time long enough to form aqueous phase containing fraction rich in calcium-sensitive pectin; (iii) passing separated extraction liquid to heat-exchanger; (iv) removing water from extraction liquid in evaporator; (v) precipitating calcium-sensitive pectin; (vi) drying and breakage. Another embodiment of the method comprises: (i) first extraction step consisting in contacting vegetable raw material with low-acidic solution having pH not higher than 4.0 and not lower than 2.5 at upper-limit temperature 90°C and lower-limit temperature above 70°C over a period of time long enough to remove calcium-insensitive pectin; (ii) separating first extraction liquid from vegetable raw material; (iii) contacting separated vegetable raw material with aqueous acid solution, more acidic than that in the step (i), at temperature and over a period of time sufficient to remove calcium-sensitive pectin fractions; (iv) separating second extraction liquid from vegetable material and passing first and second extraction liquids to heat-exchanger; (v) removing water from extraction liquids in evaporator; (vi) precipitating calcium-sensitive pectin and precipitating calcium-insensitive pectin; and (vii) drying and breakage. Aqueous composition used in food, cosmetic, and medicine-destination products contains calcium-insensitive pectin having pH above 2.5 and containing less than 2 wt % alcohol. Variant of aqueous composition contains calcium-sensitive pectin having pH below 2.2 and above 1.6 and containing less than 2 wt % alcohol. Peal composition contains peal remaining after removal of calcium-insensitive pectin obtained by treating starting vegetable material with low-acidic solution having pH not higher than 4.0 and not lower than 2.5 at upper-limit temperature 90°C and lower-limit temperature above 70°C, which composition is characterized by elevated ratio between amounts of calcium-sensitive pectin and sum of calcium-sensitive pectin and calcium-insensitive pectin.

EFFECT: simplified process and lowered expenses.

54 cl, 3 dwg, 2 tbl, 2 ex

FIELD: pectin production.

SUBSTANCE: method involves hydrolysis-extraction of pectin by cavitational treatment of pectin-containing raw material and water mixture in hydroacoustic extractor-disintegrator; separating pulp into liquid and solid phases in centrifugal force field; additionally cleaning pectin-containing extract by microfiltration process; concentrating pectin-containing extract cleaned from suspension substances by microfiltration procedure; additionally condensing cleaned pectin solution in vacuum evaporation apparatus and drying concentrate; before hydrolysis-extraction process, washing pectin-containing raw material from soluble substances ballast relative to pectin by water having temperature of 15-50 C until concentration of soluble substances in washing water is reduced by about 0.5%; providing pectin hydrolysis-extraction procedure at temperature of 30-100 C, pH value of 1.2-4.0, and process time of 60-180 min; separating pulp into liquid and solid phases in centrifugal force field at acceleration value of at least 3000 G, additionally cleaning liquid phase with suspension content not in the excess of 0.2% by weight thereof by microfiltration method with the use of membranes having average pore sizes of 0.4-1.0 micron at liquid flow rate of 1.0-5.0 m/s through channel between membranes, operating pressure of 0.1-0.8 MPa and process temperature of 20-60 C. Concentration and partial cleaning of pectin-containing extract from low-molecular soluble substances is provided by ultrafiltration process with the use of membranes having average pore sizes of 500-2,000 at liquid flow rate of 0.2-6.0 m/s in channel defined between membranes, operating pressure of 0.1-1.0 MPa, and process temperature of 20-60 C until pectin concentration in solution is at least 3.0%. Pectin-containing solution is additionally cleaned from low-molecular soluble substances ballast relative to pectin by diafiltration process with the use of membranes having average pore sizes of 500-2,000 at liquid flow rate of 0.2-6.0 m/s through channel defined between membranes, operating pressure of 0.1-1.0 MPa, and process temperature of 20-60 C until residual concentration of solution substances ballast relative to pectin is 10% or less by total content of soluble dry substances of extract. Cleaned pectin-containing solution is additionally condensed in vacuum-evaporation apparatus at temperature of product below 70 C until pectin concentration is at least 7%.

EFFECT: uniform composition of pectin fraction and increased extent of cleaning thereof from ballast substances.

7 cl, 3 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes complexes of pectin biopolymer with dicarboxylic acids of the general formula (I):

wherein R means hydrogen atom (H), methyl group (Me); m = 18-50; a) X means -(CH2)2 or b) X means -CH=CH, and a method for preparing complex of pectin with dicarboxylic acid of the general formula (I). Method involves interaction of pectin aqueous solution of the formula (II):

wherein R means hydrogen atom (H), methyl group (Me); n = 98 heated to temperature 55-60°C with dicarboxylic acid - succinic or fumaric acid at heating taken in the amount 0.13-0.55 g of acid per 1 g of pectin, and formed complex is precipitated with ethyl alcohol and dried. Prepared complexes show less toxic effect and irritating effect on stomach mucosa as compared with free succinic and fumaric acids.

EFFECT: improved preparing method, improved and valuable properties of complexes.

2 cl, 3 ex

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for isolating pectin from the vegetable raw. Method for isolating pectin from sunflower heads involves their milling, denaturation of proteins by heating, hydrolysis-extraction of solid phase, separation of liquid phase and its concentrating and drying. Extraction with dimethylformamide is carried out before hydrolysis-extraction stage followed by extraction with liquid carbon dioxide under above atmosphere pressure. The second extract is separated without change of pressure followed by abrupt drop of pressure over the solid phase up to atmosphere value and feeding the solid phase to hydrolysis-extraction stage. Invention provides improving safety due to exclusion contact of toxic solvent with the end product, reducing time process of hydrolysis-extraction stage and reducing loss of pectin substances.

EFFECT: improved isolating method.

FIELD: vegetable raw technology.

SUBSTANCE: invention relates to a method for preparing 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 successively with acetone and mixture of liquid acetylene and carbon dioxide taken in the mass ratio acetylene : carbon dioxide from 3:7 to 7:3, respectively, under the above atmosphere pressure. The second extract is separated without the pressure change followed by abrupt dropping pressure over a solid phase 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 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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