Method of producing low-molecular pectin

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.

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

 

The invention relates to methods of producing low-molecular pectin and can be used in various branches of industry and medicine, in particular in the pharmaceutical industry to create new therapeutic and prophylactic agents and low-molecular adsorbents.

Pectins are high molecular weight natural polymers. They are present in all flowering plants, included in the primary cell walls and middle lamellae. The basis of pectin molecules is poly-D-galacturonic acid. Part of the residues of D-galacturonic acid in pectin is in the form of methyl esters. If the proportion of such residues is less than 50%, the pectin is netcoalition. Fully deesterification, i.e. not containing methyl esters or containing a small quantity of pectin is also known as pectic acid.

In studies of the biological activity of pectins found a number of pharmacological effects in the low-molecular pectin derivatives - oligoglycosides. In this regard, of particular interest are oligosaccaride with a degree of polymerization of from 6 to 25-30 monosaccharide residues, which corresponds to the molecular mass of from 1 to 4.5-5 kDa. This group oligoglycosides found immunomodulatory, in erfaren-inducing, the macrophage-activating and anti-tumor activity (Kumazawa Y., Mizunoe K., Y. Otsuka Immunostimulating polysaccharide separated from hot water extract of Angelic acutiloba Kitagawa (Yamato tohki) // Immunology. 1982. Vol.47. P.75-83.). In addition, these oligosaccharides stimulate the apoptosis of colon cancer in humans (Olano-Martin, E., Rimbah GH, Gibson G.R., R.A. Rastall Pectin and pectic-oligosaccharides induce apoptosis in in vitro human colonicadenocarcinoma cell // Anticancer Res. 2003. Vol.23. P.341-346.).

It is established that oligosaccaride with a degree of polymerization of not less than 6-9 capable of forming stable complexes with ions of many heavy metals such as lead, mercury, cadmium, and others (Kohn R is divalent Binding of cations to oligomeric fragments of pectin // Carbohydr. Res. 1987. Vol.160. P.343-353.). This opens up the prospect of creating on the basis of oligoglycosides effective means for deducing from an organism of humans and animals deposited forms of these toxic elements, because due to the small molecular mass oligosaccaride can quite easily be absorbed in the gastrointestinal tract, and then excreted from the body through the kidneys.

Receiving low-molecular pectin (oligoglycosides) is usually carried out by depolymerization of natural high-molecular pectin. This can be used a number of methods. The most known is the method of enzymatic hydrolysis of pectins with pectinase. Thus, in 1944, was proposed pic is b obtain D-galacturonic acid by enzymatic hydrolysis of pectin (U.S. Pat. U.S. No. 2338534, publ. 04.01.1944 year).

A method of obtaining a composition oligoglycosides, have antibacterial properties, by enzymatic hydrolysis of pectin (IP 10226701 (A), from 08 In 37/00, publ. 25.08.2010,). According to this method, the pectin is first subjected to preliminary hydrolysis in aqueous solution at 80-100C, and then spend the final hydrolysis mixture with pectinase. The resulting product contains a mixture of saturated and unsaturated (having a double carbon-carbon linkages in the molecules in the oxidative degradation) oligoglycosides with degree of polymerization from 2 to 15 (of 0.4 and 2.7 kDa).

The disadvantage of this method is that for successful implementation of enzymatic hydrolysis is required, as a rule, certain pre-processing of pectin, for example, as in this case, partial depolymerization and deesterification during the pre-hydrolysis. Another significant drawback of enzymatic hydrolysis is that because of the specific actions pectinolytic enzymes in the obtained hydrolysates always dominated by mono-, di - and trisaccharide, and the proportion of molecules with a mass of 1 kDa (which corresponds to a polymerization degree of 6) and more insignificant.

Another known method is a method of alkaline depolymerization of pectin (EP 0487340 (A1), AR 1/08, publ. 27.05.9). According to this method, the suspension of pectin in 60% vol. isopropanol is treated three times (the chemical equivalent of the galacturonic acid) amount of sodium hydroxide for 5 days at 25C or 2 days at 40C, followed by the separation of the product on the filter, neutralization and drying. The resulting product contains pectin with a molecular mass of from 2 to 20 kDa and is intended as an excipient in cooking.

The disadvantage of this method is the large processing time and a large variation of the molecular masses of pectins in the product, as well as the fact that the galacturonic acid is unstable in an alkaline environment and readily decompose with the formation of unsaturated, eleotronic and sildopanai compounds (Kertesz Z.I. The pectic substances. Interscience Publishers, Inc., N.Y., L., 1951, 576 R.).

There is also known a method of hydrolysis of pectin at high temperature (WO 2009/004153, SW 37/06, publ. 08.01.2009). According to this method, a 1% solution of pectin with a pH of 4-5 is heated under pressure at 110C for 30-60 minutes, then the solution is cooled, the precipitated oligosaccaride with isopropanol and dried. The resulting product consists of 95% oligoglycosides with degree of polymerization 4-11 (0,7-2 kDa).

The disadvantage of this method is that at temperatures over 100C dramatically speeds up the process of thermal decomposition oligoglycosides - breaks Piran the testing cycle, oxidation, decarboxylation, formation of furfural and its derivatives. This is accompanied by a decrease in the output oligoglycosides and pollution of the hydrolyzate products of their decomposition (Kertesz Z.I. The pectic substances. Interscience Publishers, Inc., N.Y., L., 1951, 576 p.). From a chemical point of view, oligosaccaride having in the molecular structure of the products of thermal degradation of the galacturonic acid, can not fully be considered oligosaccaride.

The known method of depolymerization of polyuronides of alginates and pectins using the oxidant is hydrogen peroxide (U.S. Pat. USA US 2002/0016453 (A1), SW 37/06, publ. 07.02.2002). According to this method pechova acid in the form of pectate lithium is oxidized by hydrogen peroxide concentration of about 2% in the presence of ferric sulfate for 4 hours. Then oligosaccaride precipitated with acetic acid, washed with propanol and dried. The average degree of polymerization oligoglycosides - 16 (or 2.8 kDa). The product yield is 38%.

The disadvantages of this method include, firstly, the low yield of product. Secondly, the hydrogen peroxide simultaneously with the depolymerization of pectin causes significant destruction of the remnants of the galacturonic acid decarboxylation, breaks pyranose cycle, oxidation of the alcohol groups, and, as noted in the previous example, the resulting products can not fully midrange is to be oligosaccaride (Kertesz Z.I. The pectic substances. Interscience Publishers, Inc., N.Y., L., 1951, 576 p.).

The closest to the technical nature of the claimed method is a method of obtaining low molecular weight pectin (oligoglycosides) from flax pectin by acid hydrolysis (Bedouet L., Courtois C., Courtois J. Methods for obtaining neutral and acid oligosaccharides from flax pectins // Biotechnol. Lett. 2005. Vol.27. P.34, 36, table 1 and table 37). The method is as follows. From a sample of pectin mass of 50 mg, containing 22.9 mg (45.8%) of uronic the galacturonic acids, preparing an aqueous solution of pectin concentration of 5 mg/ml (0.5%). Then add 12 M hydrochloric acid solution to a concentration of 100 mm (0.1 g-EQ/l) and carry out the hydrolysis at 80C for 24 hours the resulting hydrolyzate is cooled to room temperature. The liquid phase containing the low-molecular products of hydrolysis, is separated from the high molecular polygalacturonic acid by centrifugation at 4C and a relative centrifugal acceleration of 20,000 g for 30 minutes. Then low-molecular products of hydrolysis - oligosaccaride - precipitated from the liquid phase with isopropanol and separated by centrifugation. The average degree of polymerization oligoglycosides - 15 (2,6 kDa). Output oligoglycosides is 33,9% of the initial content of the galacturonic acid.

A significant disadvantage of this method is the low initial concentration of pectin in plants is the op. The result is, first, the low rate of hydrolysis, as she continued constant of hydrolysis is proportional to the concentration of pectin in the solution. Secondly, the low initial concentration of pectin results in a corresponding low concentration of the final product in a ready hydrolysate - content oligoglycosides ready hydrolysate obtained by the method described above is only 0,78 mg/ml for 24 hours of hydrolysis (the yield is calculated by multiplying the initial concentration of pectin in the solution on the relative content of the galacturonic acid in pectin and the relative output galacturonic and respectively 5 mg/ml 0,458 0,339=0,78 mg/ml). And this, in turn, leads to higher unit production cost of a unit mass of product. In this case, for example, costs associated with thermoregulation for a long time the total volume of hydrolyzed at 80C and a flow rate of acid hydrolysis.

Obstacle to a significant increase in the concentration of pectin in the solution is the fact that high molecular weight pectins already at a concentration of about 1% form a sufficiently viscous solutions and the use of more concentrated solutions of pectin can create certain technological difficulties. High viscosity solutions at low concentrat the s form almost all commercial pectins, as it is with this ability is closely connected with one of the main directions of their use as thickeners and structuring agents in the food industry. For example, the viscosity of a 1.5% solution of the most common commercial pectin - Apple and citrus (producer - Herbstreith &Fox KG, Germany) is 25 to 30 times the viscosity of water.

Another disadvantage is the low technological efficiency of the method, which leads to a low yield of product. Yield - oligoglycosides is about 34%, 33% is the remainder of macromolecular polygalacturonic acid and 33% loss oligoglycosides due to their structural degradation. Thus, loss of the product is almost the same value as its output.

Technological disadvantage is that the separation of the liquid phase containing the finished product requires very strict conditions: the relative centrifugal acceleration 20000 g for most industrial centrifuges and separators either unattainable or close to their maximum operating mode, the necessity of cooling to 4C also creates additional technical problems and leads to higher process.

The goal of the invention is to obtain a low molecular weight, pecti is a, enriched fraction oligoglycosides with a molecular mass of 1-5 kDa, increasing the yield of the target product, simplify and reduce the cost method.

This objective is achieved in that in the known method of obtaining low molecular weight pectin (oligoglycosides), including the hydrolysis of pectin in an aqueous solution of mineral acid under heating, followed by the separation of the liquid phase from the insoluble residue of pectin, a selection from her low-molecular products of the hydrolysis of pectin by precipitation with an organic solvent miscible with water, according to the invention, as a feedstock for hydrolysis using viscoelastically pectin with a degree of esterification of not more than 30%, the hydrolysis of lead in cycles, with one cycle calculated by the formula:

where T is the time for one cycle, h;

C - concentration of the acid is 0.1 to 2.0 g-mol/l;

t - temperature process: 70-100C;

K - coefficient of proportionality, the values of which are within 12-18;

before deposition of low molecular weight products of the hydrolysis of pectin organic solvent liquid phase is neutralized to a pH of at least 4.0. After deposition of the obtained low-molecular products of the hydrolysis of pectin is dried.

Use as feedstock for GI is rolisa nizkoenergeticheskogo pectin with a degree of esterification of not more than 30%, with limited expansion in the acidic environment, allows the process of acid hydrolysis in heterophase system - suspension: gel nizkoenergeticheskogo pectin (solid phase) is the solution of mineral acid (liquid phase)that, firstly, allows in practice to increase the concentration of pectin in suspension up to 5-15% (calculated on the dry matter of pectin). The use of such high compared to the prototype, the concentrations of the feedstock under other equal conditions (at the same degree of hydrolysis of pectin) allows to obtain hydrolysates with correspondingly large percentage of the final product - oligoglycosides, which significantly reduces the unit cost of production of a unit mass of product. And, as a consequence, leads to the simplification and cheapening of the process of obtaining the target product.

Secondly, the hydrolysis of pectin in heterophase system allows the process is cyclic, makes it possible to fully utilize the raw materials and to prevent degradation oligoglycosides in the liquid phase, thereby increasing the yield of the target product and lowering the unit cost of its receipt.

With increasing degree of esterification of more than 30% there is a sharp increase in the volume of the swollen gel pectin and a significant reduction in its mechanical strength, which somastanozolol subsequent separation of the pectin gel from the liquid phase, it is also possible to introduce high-molecular pectin in the liquid phase.

For carrying out the proposed method can be used for virtually any commercial pectin. For this purpose, we first conduct a decrease in its degree of esterification to the required size in the range 0-30%, using any of the known methods of deesterification: alkaline, acidic or enzymatic. The most convenient and cost-effective, according to the authors, can be considered a method of alkaline deesterification pectin in a medium of an organic solvent, for example ethanol or isopropanol. This method is provided below, in the description of the implementation of the proposed method.

Use to calculate the time of hydrolysis of pectin formula (I), developed by the authors, allows the specified temperature range (70-100C), acid concentration (0.1 to 2.0 g-mol/l) and the coefficient of proportionality (K=12-18) with satisfactory accuracy to calculate the time of one cycle of hydrolysis required to obtain a product with the highest relative content of fractions oligoglycosides 1-5 kDa.

The study authors heterophase acid hydrolysis nizkoenergeticheskogo pectin was found that oligosaccaride with a molecular mass of 1-5 kDa formed during the hydrolysis of pectin, almost completely transformed into plants is the PR - the liquid phase, while the share of such molecules remaining in pectin gel-solid phase does not exceed 1-2% of their total number. Thus, an important advantage of the proposed method heterophase acid hydrolysis nizkoenergeticheskogo pectin is effective and continuous molecular separation occurring naturally in the course of the hydrolysis.

The combination in this way the effect of interfacial molecular separation and technological ease of separation of the phases allows to stop the process of hydrolysis at the right time, quickly separate the liquid phase containing the finished product, and then spend the next cycle of hydrolysis of the remaining high-molecular pectin.

These limits of temperature and acid concentration are associated primarily with economic and technological reasons. Thus, when the air temperature is below 70C and an acid concentration below 0.1 g-mol/l is a significant decrease in the rate of hydrolysis of pectin and a significant increase of the process time, this leads to increased cost of production of the target product.

At temperatures over 100C dramatically speeds up the process of thermal decomposition oligoglycosides - breaks pyranose cycle, oxidation, decarboxylation, formation of furfural and E. what about the derivatives. This is accompanied by a decrease in the output oligoglycosides and pollution of the hydrolyzate products of their decomposition. The increase in acid concentration of more than 2.0 g-mol/l does not provide a significant increase in the rate of hydrolysis, but leads to a significant waste acid and additional costs for subsequent neutralization and release of product from the resulting salts, which, ultimately, leads to the complication of the process of obtaining the target product.

Neutralization of the liquid medium to a pH of at least 4.0 before deposition of low molecular weight products of the hydrolysis of pectin organic solvent provides the receiving sludge of low molecular weight pectin (oligoglycosides) with optimal consistency - thick, well-separated from the liquid phase. At pH below 4.0 is an increase in specific volume of sediment and the weakening of its structure, and, consequently, difficult separation of the precipitate from the liquid phase.

As the mineral acid can be used, in particular, hydrochloric, sulphuric, nitric acid.

As the organic solvent can be used known organic solvents, miscible with water, in particular acetone, propanol, isopropanol, ethanol, methanol.

Separating the liquid phase from the insoluble sludge can be maintained either by filtering or centrifugual is of relatively small magnitude of the centrifugal acceleration 500-1000 g. This significantly reduces the cost and simplifies the process of obtaining the target product in comparison with the prototype, as in the prototype, the centrifugation is carried out at the acceleration of 20,000 g and 4C.

From an economic point of view it is advisable to maintain the hydrolysis of pectin in a constant process conditions, i.e. at a constant amount of pectin in the reaction environment, to make new additive servings of raw materials to the rest of the pectin after separation of the liquid phase to compensate for its consumption in the course of the hydrolysis. This allows any number of consecutive identical cycles of hydrolysis and to obtain any required number of the target product with the desired molecular weight, 1-5 kDa.

Raw materials can be added to the balance of pectin after each or after several cycles of hydrolysis, and its amount can be calculated either by a volume change of the gel pectin, or number of pectin remaining after separation of the liquid phase.

In the first case, to determine the amount of added material volume change of the gel pectin, take a certain amount of pectin (m1), mineral acid is added before the formation of the suspension and before hydrolysis, the suspension of pectin in the mineral acid is centrifuged at a relative centrifugal acceleration of 500-1000 g for 5-15 minutes and record the initial volume of the gel - pectin, V1, Jr. And before subsequent cycles of hydrolysis of the rest of the pectin after hydrolysis centrifuged in the same conditions with the same amount of relative centrifugal acceleration and time, fixing V2- amount of residual pectin after hydrolysis, Jr.

To determine the amount of the added raw material by volume of residual pectin after centrifugation it is calculated by the formula:

where m is the mass of the added raw materials, g;

m1- weight of the feedstock, g;

V1- the initial volume of the swollen material - gel nizkoenergeticheskogo pectin, ml;

V2- amount of residual pectin after hydrolysis, Jr.

Use for calculation of the formula (II), proposed by the authors, allows with sufficient accuracy to determine the mass of the added raw materials, which restores the content of pectin to the initial concentration. Ultimately, this ensures maximum use of residual pectin, increase the yield of the target product and the possibility of obtaining it in sufficient quantity.

In the second case, to determine the amount of the added raw materials for the quantity of pectin, remaining after separation of the liquid phase, before starting the process of hydrolysis record the mass of the feedstock, m1also determine it nigerianisation acid, C1. At the end of time of hydrolysis, calculated by the formula (I), separating the rest of the pectin from the liquid phase, record its mass m2determine the content of the galacturonic acid With2.

The number of added raw materials are calculated according to the formula:

where m is the mass of the added raw materials, g;

m1- weight of the feedstock, g;

m2the mass balance of pectin after separation of the liquid phase, g;

C1- the content of the galacturonic acid in the feedstock, %;

With2- the content of the galacturonic acid residue pectin, %.

Formula (III), proposed by the authors, as well as the formula (II), allows to accurately determine the amount of added material.

To determine the content of the galacturonic acid in the feedstock, and the rest of the pectin may be used any of known methods, such as titrimetric (Afanas'ev, S. p., f.chirva V.Y., kazawa GN. and other Modified titrimetric methods of analysis of pectin Chemistry natures. connections. 1984. No. 4. S-431.) or photometric (Blumenkrantz n, Asboe-Hansen G. New method for quantitative determination of uronic acids // Anal. Biochem. 1973. Vol.54. P.484-489). Given that during each cycle of hydrolysis consumes approximately the same amount of raw materials, there is no need to calculate the number of the added raw materials after the each cycle of hydrolysis - enough to hold them every 5-10 cycles.

The method is as follows.

Example 1

Take 30.0 g pectic acid (Serva, No. 31680) with the content of the galacturonic acid 82.2% degree of esterification of less than 1% and mixed with 200 ml of hydrochloric acid concentration of 0.1 g-mol/l (C). Received 15%, the suspension is heated to 100C (t) in a boiling water bath and maintained at this temperature and stirring for a time (T)calculated by the formula (I) when the coefficient of proportionality K=18:

Then the suspension is cooled and filtered to filter the suspension using polypropylene filtrating PL-30 (LOSMA, Italy). The remainder of pectin on the filter is washed with 200 ml of hydrochloric acid concentration of 0.1 g-mol/l (C) for a more complete separation oligoglycosides. To the residue add pectin solution of hydrochloric acid concentration of 0.1 g-mol/l to restore the original volume of the suspension. The rest of the pectin resuspended in the liquid phase and carry out the next cycle of hydrolysis in the same terms - T=4,1 hours at t=100C. Just spend 5 cycles of hydrolysis, each time separating and washing the residue of pectin as described above. The total amount of the obtained filtrate is 1440 ml, content oligoglycosides - 8,23 mg/ml

The liquid phase (filtrate) to neutralize the H 4,0 5,0 M solution of sodium hydroxide and the precipitated oligosaccaride adding 4.3 liter of ethanol. The mixture is intensively stirred for minutes, and then, after 12 hours, the precipitation oligoglycosides separated by centrifugation at OTSU 1000-1500 g for 15 minutes and dried at 80C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 13,38 g (content oligohaline sodium clean the galacturonic acid is 88.5%). To determine the relative (in stock) product yield, in terms of galacturonic acid, install the consumption of raw materials by the difference between the total number of pectic acid used for hydrolysis (30.0 g), and the amount of pectin remaining after hydrolysis. For the amount of pectic acid recalculate the content the galacturonic acid, and balance of pectin determine the total content of the galacturonic acid photometric method. Installed the consumption of raw materials is on the galacturonic acid 13,30, the Relative yield on the galacturonic acid are, respectively, of 89.1%. According to exclusive chromatography of the resulting product in 0.05 M acetate buffer with a pH of 3.0 on a column of Sephadex G-50 superfine calibrated using a standard set of pullulan, the relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 62.5%.

Example 2

Take 10.0 g pectic acid (Serva No. 31680) (m 1) with the content of the galacturonic acid 82.2% degree of esterification of less than 1% and mixed with 200 ml of hydrochloric acid concentration of 0.1 g-mol/l (C)record the volume received 5% suspension - it is 210 ml, then the suspension is centrifuged for 15 minutes at a relative centrifugal acceleration (OTSU) 500 g and record the initial volume of the gel pectin - he is 48 ml (V1). The precipitate pectin gel resuspended in the liquid phase, heated to 100C (t) in a boiling water bath and maintained at this temperature and stirring for a time (T)calculated by the formula (I) when the coefficient of proportionality K=18:

Then the suspension is cooled to room temperature and centrifuged for 15 minutes at OTSU 500 g. The liquid phase is separated from the precipitate gel pectin, measure the amount of sludge is 40 ml (V2). Substituting the obtained data on the original volume nizkoenergeticheskogo gel pectin (V1) and the rest of the pectin gel after hydrolysis (V2), equal to 40 ml, in the formula (II), calculate the required additive raw material (m) to restore the original amount of pectic acid:

To the precipitate add the specified amount of pectic acid and a hydrochloric acid concentration of 0.1 g-mol/l (C) - to the East is Stanovlenie the initial volume of the suspension. Sediment resuspended in the liquid phase and carry out the next cycle of hydrolysis in the same conditions of 4.1 hours at 100C. Just spend 5 cycles of hydrolysis. Each time after separation of the liquid phase measured volume of sediment pectin: if it remains constant (equal to 40 ml (V2)), the amount of raw materials that are added to the residue pectin, also remains constant of 1.65 g (m), because the amount of sediment pectin during hydrolysis was not changed (if the amount of sludge varies, according to the formula (II) re-calculate the necessary Supplement of raw materials). The volume of the resulting supernatant liquid phase is 810 ml, content oligoglycosides - 7,15 mg/ml of the Liquid phase is neutralized to a pH of 4.0 to 5.0 M solution of sodium hydroxide and the precipitated oligosaccaride the addition of 2.4 liters of acetone. The mixture is intensively stirred for minutes, and then, after 12 hours, the precipitation oligoglycosides separated by centrifugation at OTSU 1000-1500 g for 15 minutes and dried at 80C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 6,53, the Relative yield on the galacturonic acid, defined as described in the previous example, is to 88.3%. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 62,0%.

Example 3

Get viscoelastically pectin controlled by the alkaline deesterification vysokotarifitsirovannyh pectin.

Take 50 g vysokotarifitsirovannyh citrus pectin (Herbstreith &Fox KG, Germany) suspended in 0.5 l of 60% vol. ethanol and gradually added in several portions 5.0 M solution of sodium hydroxide, controlling the degree of esterification of pectin in samples taken after adding each portion of sodium hydroxide. After reaching the value of the degree of esterification of less than 30% to the suspension, add 20 ml of concentrated hydrochloric acid (density d=1.19 g/cm3), pectin is separated by filtration, washed with 150 ml of 50% ethanol and dried at 80C. the Output nizkoenergeticheskogo pectin - 47 g, the content of the galacturonic acid - 74,8%, the degree of esterification by 30.0%.

Take 10.0 g obtained nizkoenergeticheskogo pectin (m1), mixed with 200 ml of hydrochloric acid concentration of 0.5 g-mol/l (C) and record the volume received 5% suspension - it is 210 ml, then the suspension is centrifuged 5 minutes at OTSU 1000 g and record the initial volume of the gel pectin - he is 112 ml (V1). The precipitate pectin gel resuspended in the liquid phase and thermostatic at 80C (t) and constant stirring during the time (T)calculated by the formula (I) when the coefficient of proportionality K=12:

Then the suspension is cooled to room temperature and centrifuged 5 minutes at OTSU 1000 g. The liquid phase Department of the Ute from the precipitate gel pectin, and the residue is washed twice with a solution of acid for a more complete separation oligoglycosides: the residue is suspended in 100 ml of hydrochloric acid concentration of 0.5 g-mol/l (C), then centrifuged 5 minutes at OTSU 1000 g, the liquid phase is drained and repeat the flushing of sediment. After washing the measured volume of sediment pectin after hydrolysis he is 96 ml (V2). Substituting the obtained values of V1V2and m1in the formula (II), calculate the required additive raw material (m) to restore the original amount of pectin:

To the precipitate add the specified number nizkoenergeticheskogo pectin (1,43 g) and a solution of hydrochloric acid concentration of 0.5 g-mol/l (C) to restore the original volume of the suspension. Sediment resuspended in the liquid phase and carry out the next cycle of hydrolysis in the same conditions of R=7.0 hours at t=80C. Just spend 5 cycles of hydrolysis. Each time after separation of the liquid phase measured volume of sediment: if it remains constant (equal to 96 ml), the amount of raw materials that are added to the residue pectin, also remains constant 1,43 g, if the amount of sludge varies, according to the formula (II) re-calculate the necessary Supplement of raw materials. The volume of the resulting supernatant liquid phase - 1450 ml, content oligoglycosides - of 3.48 mg/ml of the Liquid phase is neutralized first with dry sodium hydroxide to a pH of 1-2, then a 5.0 M solution of sodium hydroxide to a pH of 6.0. Oligosaccaride precipitated by the addition of 4.5 l of ethanol. The precipitation oligoglycosides separated by centrifugation for 15 minutes at OTSU 1000-1500 g, then cleaned from salts: resuspended in 0.6 l of 70% ethanol and re-centrifuged. The wet precipitate is dried at 80C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 5,70, the Relative yield on the galacturonic acid, defined as described in the previous example, is 94.2 percent. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 67,0%.

Example 4

Take 30 g of pectic acid (see example 1) (m1) with the content of the galacturonic acid and 82.2% (C1), mixed with 200 ml of a sulfuric acid concentration of 2.0 mol/l (C) and record the volume received 15% of the suspension - it is 230 ml Suspension thermostatic at 70C (t) and constant stirring during the time (T)calculated by the formula (I) when K=12:

Then the hot suspension is filtered, the filter suspension use polypropylene filtrating PL-30 (LOSMA, Italy). The remainder of pectin on the filter is washed with 200 ml of a sulfuric acid concentration of 2.0 mol/l (C) for a more complete separation oligoglycosides. The resulting filtrate is cooled on the room temperature. The rest of the pectin weigh and determine in it the percentage of the galacturonic acid by titrimetric method. On the obtained values of the mass balance of pectic acid - 127,1 (m2and the content of the galacturonic acid - 16,0% (C2) are calculated according to the formula (III) additive raw material (m) to restore the original amount of pectic acid:

To the residue pectin add the calculated amount of pectic acid (m) and a solution of sulfuric acid concentration of 2.0 mol/l (C) to restore the original volume of the suspension. The rest of the pectin resuspended in the liquid phase and carry out the next cycle of hydrolysis in the same terms - T=7.5 hours at t=70C. Just spend 5 cycles of hydrolysis. Each time after separation of the liquid phase remaining pectin weighed again, define it, the percentage of the galacturonic acid and formula (III) calculate the required additive raw materials. The total amount of the obtained filtrate is 1280 ml, content oligoglycosides to 16.4 mg/ml of the Filtrate is neutralized: first dry sodium hydroxide to pH 1-2, and then a 5.0 M solution of sodium hydroxide to pH 8. Oligosaccaride precipitated by the addition of 4.0 l of isopropanol. The precipitation oligoglycosides separated by centrifugation for 15 minutes at OTSU 1000-1500 g, then the sight is up from salts: resuspended in 2.0 l of 70% isopropanol and re-centrifuged. The wet precipitate is dried at 80-100C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 23,75, the Relative yield on the galacturonic acid is 95,1%. The relative content of fractions oligoglycosides 1-5 kDa is 62,7%.

Example 5

Get viscoelastically pectin. To do this, in 0.5 l of 50% ethanol diluted to 20.0 g of sodium hydroxide, then with stirring 100.0 g vysokotarifitsirovannyh citrus pectin (Herbstreith &Fox KG, Germany). The mixture is stirred for 50 minutes, then gradually in small portions add 40,0 ml of concentrated hydrochloric acid, pectin is separated by filtration, washed with 300 ml of 50% ethanol and dried at 80C. the Output nizkoenergeticheskogo pectin - 93,3 g, the content of the galacturonic acid - 76,5% (C1), the degree of esterification is 0%.

Take 20,0 g (m1) received nizkoenergeticheskogo pectin is mixed with 200 ml of a solution of nitric acid concentration of 0.5 g-mol/l (C) and record the volume received 10% suspension - it is 220 ml Suspension thermostatic at t=90C and stirring for a time (T)calculated by the formula (I) when K=14,5:

After hydrolysis, the suspension is cooled and filtered to filter the suspension using polypropylene filtrating PL-30. The rest of the pectin is and the filter washed with 150 ml of nitric acid concentration of 0.5 g-mol/l (C) for a more complete separation oligoglycosides. To the residue add pectin solution of nitric acid concentration of 0.5 g-mol/l (C) to restore the original volume of the suspension. The rest of the pectin resuspended in the liquid phase and carry out the next cycle of hydrolysis in the same conditions - 3.0 hours (T) at 90C (t). Just spend 3 cycles of hydrolysis. The washed residue of pectin after the last cycle of hydrolysis weigh and determine in it the percentage of the galacturonic acid by titrimetric method. On the obtained values of the mass balance of pectin - 56,1 g (m2and the content of the galacturonic acid - 16,4% (C2) are calculated according to the formula (III) additive raw material (m) to restore the original amount of pectin:

To the residue add pectin specified number nizkoenergeticheskogo pectin and conduct the following 3 cycles of hydrolysis in the same conditions. The total amount of the obtained filtrate is 1660 ml, content oligoglycosides - for 6.81 mg/ml of the Filtrate is neutralized: first dry sodium hydroxide to pH 1-2, and then a 5.0 M solution of sodium hydroxide to a pH of 5. Oligosaccaride precipitated by the addition of 5.0 l of ethanol. The precipitation oligoglycosides separated by centrifugation for 15 minutes at OTSU 1000-1500 g, then cleaned from salts: resuspending 1.3 l of 70%. ethanol and re-centrifuged. Wet the residue is dried at 80C. The output product is a dry powder of oligoamenorrhea sodium - 12,77, the Relative yield on the galacturonic acid is 92,5%. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 65,0%.

Example 6

Get viscoelastically pectin.

In 0.4 l of 50%. isopropanol was dissolved 20 g of sodium hydroxide, is then added with stirring 100 g vysokotarifitsirovannyh Apple pectin (Herbstreith &Fox KG, Germany). The mixture is stirred for 10 min, then gradually in small portions add 40 ml of concentrated hydrochloric acid, pectin is separated by filtration, washed with 300 ml of 50% isopropanol and dried at 80-100C. the Output nizkoenergeticheskogo pectin - 94,5 g, the content of the galacturonic acid - 78,4% (C1), the degree of esterification was 13.8%.

Take 20 g of the obtained nizkoenergeticheskogo pectin (m1), mixed with 200 ml of a sulfuric acid concentration of 1.0 mol/l (C) and record the volume received 10% suspension - it is 220 ml Suspension thermostatic at t=90C and stirring for a time (T)calculated by the formula (I) when K=16:

Then the suspension is cooled and filtered to filter the suspension using polypropylene filtrating PL-30. The remainder of pectin in the filter, the e washed with 150 ml of a sulfuric acid concentration of 1.0 mol/l (C) for a more complete separation oligoglycosides. The rest of the pectin weigh and determine in it the percentage of the galacturonic acid by titrimetric method. On the obtained values of the mass balance of pectin - 79,0 g (m2and the content of the galacturonic acid - 15,5% (C2) are calculated according to the formula (III) additive raw material (m) to restore the original amount of pectin:

To the residue add pectin specified number nizkoenergeticheskogo pectin and a sulfuric acid concentration of 1.0 mol/l (C) to restore the original volume of the suspension. The rest of the pectin resuspended in the liquid phase and carry out the next cycle of hydrolysis in the same conditions T=2.0 h at t=90C. Just spend 5 cycles of hydrolysis. Each time after separation of the liquid phase to the residue add pectin 4.42 g nizkoenergeticheskogo pectin (m). Because in the course of hydrolysis of pectin may be some valid discrepancy between the number of added raw and real value of consumption of raw materials, to eliminate such possible differences after 5 cycles of hydrolysis again carry out the calculation of the required additives raw materials. To do this, the washed residue of pectin after the last cycle of hydrolysis weigh and determine in it the percentage of the galacturonic acid titrimetrically. On the obtained values of the mass balance of pectin - 82.8 g (m2and the content of the galacturonic acid and 15.1% (C2) are calculated according to the formula (III) required a one-time corrective additive raw material (m) to restore the original amount of pectin:

To the residue add pectin specified number nizkoenergeticheskogo pectin. Then spend the next 5 cycles of hydrolysis in the same conditions. Each time after separation of the liquid phase to the rest of the pectin still add 4.42 g nizkoenergeticheskogo pectin. The total amount of the obtained filtrate is 2720 ml, content oligoglycosides - 11,40 mg/ml of the Filtrate is neutralized: first dry sodium hydroxide to pH 1-2, and then a 5.0 M solution of sodium hydroxide to a pH of 5. Oligosaccaride precipitated by the addition of 8.0 l of isopropanol. The precipitation oligoglycosides separated by centrifugation for 15 minutes at OTSU 1000-1500 g, then cleaned from salts: resuspending 2.6 liters of 70%. isopropanol and re-centrifuged. The wet precipitate is dried at 80-100C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 35,05, the Relative yield on the galacturonic acid is 90.5%. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 67,7%.

Ka is seen from the above examples, the inventive method heterophase hydrolysis owing to the insolubility of the original pectin acid to hydrolysis purposefully to obtain a product with the desired molecular weight, and still use the original pectin almost completely, i.e. avoids any significant technological losses of raw materials and to increase the final yield of the product (on the galacturonic acid) in comparison with the prototype 2.6-2.8 times to 88-95% of the original raw materials.

In addition, in the present method, in contrast to the known method, the hydrolysis of raw materials is a separate, relatively short cycles, which can significantly limit the destruction oligoglycosides in the process of hydrolysis and, consequently, further increase the yield of the target product.

Moreover, the offered technical solution provides compared to prototype faster process and, accordingly, the reduction of unit production costs and time to production of one kilogram of product at a significant savings in raw materials, also eliminates the use of complicated and expensive process equipment to separate the liquid phase from the remainder of pectin.

1. The method of obtaining the low-molecular pectin, including the hydrolysis of pectin in aqueous solution mineral sour the s when heated, followed by the separation of the liquid phase from the insoluble residue of pectin, the release of her low-molecular products of the hydrolysis of pectin by precipitation with an organic solvent miscible with water, characterized in that as a feedstock for hydrolysis using viscoelastically pectin with a degree of esterification of not more than 30%, the hydrolysis of lead in cycles, with one cycle calculated by the formula:

where T is the time for one cycle, h;
C - concentration of the acid is 0.1-2.0 g-mol/l;
t is the process temperature of 70-100C;
K - coefficient of proportionality, the values of which are within 12-18;
before deposition of low molecular weight products of the hydrolysis of pectin organic solvent liquid phase is neutralized to a pH of at least 4.0, and after deposition of low-molecular products of the hydrolysis of pectin is dried.

2. The method according to claim 1, characterized in that after each or several cycles of hydrolysis to the rest of the pectin add a new batch of raw materials, the amount of which is calculated by the formula:

where m is the mass of the added raw materials, g;
m1- weight of the feedstock, g;
V1- the amount of pectin gel before hydrolysis, ml;
V2- amount of residual gel pectin after hydrolysis, ml,
while V1and V2determined after centrifugation of the gel pectin, or by the formula:

where m is the mass of the added raw materials, g;
m1- weight of the feedstock, g;
m2the mass balance of pectin after separation of the liquid phase, g;
C1- the content of the galacturonic acid in the feedstock, %;
With2- the content of the galacturonic acid residue pectin, %.



 

Same patents:

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.

2 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of obtaining pectine polysaccharides from waste wood and can be used in food, pharmaceutical, chemical and other industries. Siberian larch bark (Larix sibirica Ledeb.) and/or Dahurian larch bark (Gmelin) (Larix gmelinii Rupr. (Rupr.)) is prepared for complete extraction of pectine polysaccharides through successive treatment with acetylacetate, water and a solution of oxalic acid.The bark residue is then extracted with an ammonium oxalate solution at 60-70C for 3-5 hours and then concentrated. The end product is then dropped into 96% ethanol and lyophilically dried.

EFFECT: disclosed method provides high output of up to 12% of pectine polysaccharides from larch bark, having membrane stabilising activity and capable of reducing silver ions from salt solutions to nanosize particles with zero valence, where during the reaction a nanobiocomposite is formed from silver nanoparticles with particle size of 3-27 nm, which are stabilised with an amorphous matrix - pectine.

4 cl, 2 dwg, 1 tbl, 6 ex

FIELD: wood working industry.

SUBSTANCE: invention relates to method for processing of conifer bark. Method for processing of conifer bark includes bark grinding, serial extraction with hydrocarbon dissolvent and water, concentration of extract and extraction of target fractions of lipids and polyphenol. After extraction of lipids and polyphenols, remaining bark is exposed to hydrolysis-extraction with acidified water at the temperature of 70-75C, hydraulic modile 1:(2.0-2.5), for 6-7 hours, with further concentration of extract by method of ultrafiltration at the temperature of 40-47.5C and pressure of 0.4-0.45 MPa, depositing fraction of pectine substances by aliphatic alcohol, separation of pectines deposit by centrifugation and spray-drying at the temperature of 40-40.9C and pressure of 0.3-0.38 MPa. Remained extracted bark is used to produce bark compost fertilisers.

EFFECT: suggested method makes it possible to extract biologically active substances from bark to the maximum.

2 tbl, 1 ex

FIELD: medicine.

SUBSTANCE: dry powder of pectic acid or its water-soluble salt is mixed with aqueous solution of calcium salt at concentration at least 0.6 mol/l. The prepared calcium pectate is separated from aqueous phase.

EFFECT: process simplification and reduction of power inputs.

2 cl, 7 ex

FIELD: chemistry.

SUBSTANCE: proposed method of producing flax polysaccharides involves extraction in distilled water under the effect of ultrasound at 30 kHz and 182276 W/cm intensity at 2732C. Ultrasonic treatment is done in 1217 minutes. The invention simplifies the extraction process, reduces expenses and cuts on time of obtaining polysaccharides.

EFFECT: significant increase in output and quality of polysaccharide.

2 cl, 4 dwg, 4 ex

FIELD: chemistry.

SUBSTANCE: invention relates to pectin and processed initial material, which contains pectin. Method of obtaining processed initial material by deactivation of pectinesterase includes obtaining fruit vegetable material, containing pectin, and bringing it in contact with water, which has pH value from 3.2 to 3.9, at temperature ≤70°C. After that processed initial material is extracted. In addition, invention relates to use of processed initial material, containing pectin, obtained according to said method, respectively, for pectin extraction, as food for animals or as ingredient in food products. In addition invention relates to pectin, obtained according to said method, by means of extraction from initial vegetable material, molecular weight of said pectin being higher on value up to 50% than molecular weight of pectin, obtained from extraction of similar but unprocessed initial vegetable material, containing pectin. Ratio of sensitivity to calcium of said pectin and sensitivity to calcium of pectin, extracted from similar, but unprocessed with washing, initial vegetable material, which contains pectin, is within 0.90-1.40. Pectin preserves molecular weight and etherification degree well, has high output and low sensitivity to calcium.

EFFECT: obtaining method of processing vegetable material, which contains pectin, preserving molecular weight and degree of pectin etherification.

30 cl, 2 dwg, 19 tbl, 9 ex

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

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: 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.

Up!