Method of separating biologically active compounds from propolis by vacuum ultrasonic extraction
SUBSTANCE: invention relates to a method of producing dry propolis. Said method includes grinding raw material, extraction with 96% ethyl alcohol at temperature of +20-25°C using a vacuum-ultrasonic device, filtering, purification from heavy metals and other impurities using a carbon sorbent, followed by evaporation.
EFFECT: disclosed method increases output of biologically active substances and enables purification of propolis from wax, mechanical impurities, high-molecular weight substances, heavy metals and pesticides.
2 dwg, 3 tbl, 1 ex
The invention relates to medicine and perfumery industry and relates to a method of cleaning propolis from heavy metals, toxins and radioactive substances to produce organic active groups, used as medicines.
The closest to the proposed method to the technical nature, can be considered as a method of producing the alcoholic extract of propolis vacuum ultrasonic extraction (patent No. 23729280, however, he does not receive dry biologically active compounds, to prepare a standardized medicines for various applications.
The purpose of the invention is the obtaining of purified dry substance of propolis with simultaneous cleaning from heavy metals such as si, Pb, Zn, Cd) and from residues of medical drugs with toxicity used in treatment of bees and pesticides from entering the hive in the processing of agricultural land, while reducing the retrieval time of extractives and concentrating them to dry condition with moisture content of 10-12%, using for this purpose the vacuum-ultrasonic extraction continuous extraction of propolis.
The goal of obtaining a dry purified substance of propolis was achieved by grinding propolis raw �predvaritelno frozen at a temperature of 16-20°C and extraction with ethyl alcohol 96° at a temperature of 20-25°C.
In a glass vacuum ultrasonic device of continuous action, ethanolic extract of propolis treated multifunctional carbon sorbent (know-how) to remove heavy metals, radioactive substances, pesticides with high toxicity.
Purified ethanolic extract of propolis was subjected to vacuum evaporation to a moisture content of 9-12%. Finished dry substance propolis is readily soluble in saline solution. From the dry substance can be prepared standardized alcohol-dosage form, as well as to prepare ointments for medical use.
Example 1. Method for producing of dry propolis.
We have developed a simple method for pre-cleaning of propolis-raw, allowing to remove wax and contaminants (see figure No. 1). Chopped cooked propolis is loaded into glass columns No. 1 and No. 3 of 20 kg of propolis in each. The column is equipped with an ultrasonic device under No. 11 and No. 12.
Column No. 1, No. 2 and No. 3 have a diameter of 0, 2 m, height 1.2 m with filter unit above and below (#13 and # 14).
All columns are sealed. Centered within a column mounted ultrasonic device with the consuming power of 5 volts, and having a mass of 200 g, which may be included in electric network of alternating current with the help of �stantsionnogo management. Column No. 1 and No. 3 is provided above and below the multi-way opening and closing valves (No. 15). To the upper crane columns No. 1 and No. 3 is attached the vacuum hose connected to a vacuum pump (No. 9) and the bottom valve of the columns No. 1 and No. 3 is connected via a hose to a centrifugal pump (No. 10) and the lower valves of the columns No. 1 and No. 3.
From the tank (No. 6), where the prepared alcohol 96° concentration pump (No. 18) fill in the column (No. 2) 35-40 liters of ethyl alcohol, include the vacuum in the columns No. 1 and No.). In the upper part of the column (No. 1) installed a vacuum gauge (No. 19), which controls the negative pressure in the columns No. 1 and No.).
Ultrasonic device include when the temperature of ethanol will reach 20-25°C and the vacuum becomes equal to 0,9-0,95 Athy, then fill with the prepared column alcohol from the column (No. 2), open the bottom valve of the column (No. 1 and No. 2) and through the centrifugal pump through the bottom of the crane column (No. 1) regulate the flow of ethanol manually, so that the pressure in the column (No. 1) did not fall below 0.65 in Athy.
When filling out column No. 1 of the alcohol to the top of the drain fitting and the drain of the extract in column # 2, speed drain, reduce and within 1.5-2 hours to conduct the extraction at a temperature of 20-25°C in a mobile alcohol layer enabled device. This leads to increased diffusion of molecules of biologically activediary from the depths of pieces of propolis.
We achieve this reduction of resistance free path of the active compounds to the surface of the extract at low temperatures, without losing a large amount of energy for heating, thereby getting rid of the remainder of the wax and other substances in the extract. Ultrasonic device affects propolis and leads him to powder state, thereby increasing the completeness of extraction of biologically active substances. After 1,5-2 hours of extraction shut off the vacuum and ultrasonic device and under a pressure of 0.5 ATM through the bottom valve of column No. 1 of the ethanolic extract of propolis move under pressure into the container No. 4, washed the meal after extraction of propolis 5 liters of 96% ethanol through the top fitting of column No. 1, and then removed from the column propolisnoe cake to download new propolis.
In columns # 2 and # 3 are the same process operations as in column No. 1, the combined alcoholic extracts of propolis obtained by extraction in columns # 1 and # 3 act in the capacity of No. 4, equipped with a stirrer. Ethanolic extract of propolis treated multifunctional coal-sorbent (know-how) to remove from propolis heavy metals, pesticides and residues of therapeutic drugs used for the treatment of bees, which have toxicity.
2 g multifunction Corben�and add to 1 liter of alcoholic extract of propolis, stirring occasionally, for 3 hours, then filtered or separated in the separator. The obtained purified extract from tank No. 4, freed from impurities, is collected in the tank No. 5. From tank No. 5 the extract is fed to a vacuum evaporator No. 7 and under reduced pressure with the degree of dilution (0.9 to 10-1)is evaporated to the dry dilution lumps. Discharged from the evaporation vessel and dried in a vacuum Cabinet at a baking sheet at 45-50°C, adjusted to a moisture content of 9-12%. Powdered propolis in the amount of 2170,0 g packaged in one-litre pitcher glass or two-liter jars of dark glass with an airtight seal screw caps or plastic bags and tightly wrapped, removing the air.
Warranty period of storage of dry propolis is 4 years from the manufacturing date.
For comparison, I took propolis from six regions of the Russian Federation and perform the vacuum-ultrasonic extraction and purification of multifunctional sorbent.
Next, in table.1 presents the results of the microbiological purity of the dry substance of propolis, which was obtained after vacuum ultrasonic processing device described above.
Propolis taken from the Orel region (No. 1), Krasnodar territory (No. 2), Pskov oblast (No. 3), Mordovia (No. 4), Tula region (No. 5) and the Kursk region (No. 6), which are listed in the table under the solicitation�existing room: 1, 2, 3, 4, 5, 6.
|No. samples from different regions||Bacteria and fungi in total, 1 ml not more than 102||Enterobakteraceae and some other gram-negative bacteria in 1 g not more than 10-1||Pseudomonas, Aeruginaosa. Staphylococcus, Freus should be no|
All investigated samples of dry purified propolis meets the requirements of the global Fund XI, issue.2 p. 193, amendment No. 3, cat.2.
|Antimicrobial activity of dry substances of propolis obtained from six different regions of the Russian Federation.|
|Nos. of samples of regions of the Russian Federation||Antimicrobial effect Breeding 1:300 1:600 1:1200||The content of heavy metals not more than 0.001%||Note|
From the data obtained in table.2 that all of the sample inhibit the growth of test microorganisms in a dilution of 1: 300
|Results content the amount of phenolic compounds of dry purified propolis vacuum ultrasonic extraction Cm. Figure No. 2|
|No. samples of regions of the Russian Federation||Number of propolis dry cleaned, taken in grams||Number of added alcohol 80% ml||Contents. the amount of phenolic compounds, %||Note: the content of phenolic compounds 2-6%|
|1.||10||up to 1000||5,24||ACC. FS|
|2.||10||up to 1000||4,26||- "-|
|3.||10||up to 1000||Of 5.06||- "-|
|4.||10||up to 1000||4,70||- "-|
|5.||10||up to 1000||The 4.25||- "-|
|6.||10||up to 1000||4,93||- "-|
Upon receiving the dry substance of propolis with cleaning multifunction sorbitol, studies have shown that the biological activity of propolis is interconnected with the purity of identified compounds in it and, therefore, results in a higher quality dry substance and propolis tincture, relevant regulatory documents.
Thus, the developed vacuum-ultrasonic technology in a mobile alcoholic extract of receipt of propolis tincture, which increases the yield of biologically active substances, separates propolis waxes, solids, resinous lipidrich and other niskama�molecular and high-molecular substances, heavy metals and pesticides entering the propolis.
Test the microbiological purity of the dry substance of propolis was performed in accordance with the requirements of the global Fund XI, issue.2 p. 193, amendment No. 3, category 2. Microbiological purity was carried out in 6 series obtained from different regions of the Russian Federation.
Determination of phenolic compounds of propolis are presented in samples 1, 2, 3, 4, 5, 6, that speaks to the high quality of dry propolis.
Method for producing of dry propolis for the preparation of medicinal preparations containing propolis, which consists of grinding of raw material, extraction with ethyl alcohol 96% at a temperature of 20-25°C with the use of vacuum-ultrasonic device for filtration as well as purification from heavy metals and other impurities with the use of carbon sorbent and subsequent evaporation.
FIELD: engines and pumps.
SUBSTANCE: device (100, 200) for reduction of acidity of motor oil of internal combustion engines includes container (101, 202), through which certain amount of motor oil flows; with that, the container includes ion exchanger (102, 202) representing a univalent cation exchanger, and container (101, 201) that is located in motor oil flow. The invention also describes a control method of acidity of motor oil, at which oil must pass through an acidity control device according to the invention. Besides, the invention relates to a transport vehicle provided with an acidity control device of motor oil according to the invention.
EFFECT: reduction of motor oil acidity; increasing service life of oil.
11 cl, 11 dwg
SUBSTANCE: group of inventions relates to method of separating harmful substances from gas flow and deals with removal of harmful substances from carbon dioxide and device for its realization. Method of separating harmful substances from gas mixture, which mainly contains carbon dioxide CO2, as well as valuable substances such as hydrogen H2, carbon monoxide CO, nitrogen N2 or noble gas, in which CO2 condensation is realised in order to separate liquid CO2. As harmful substance hydrogen sulphide H2S or carbonylsulphide COS is processed. Adsorption separation of H2S or COS from liquid CO2 is realised. Temperature of method is set in the range from -30°C to -70°C.
EFFECT: invention provides energy-preserving possibility for removal of harmful substances in electric power plants with main heating be means of fossil fuel.
8 cl, 2 dwg
SUBSTANCE: matrix can be used in purification of proteins, where protein represents antibody, fragment of antibody or antibody-containing fused protein. Ligand corresponds to the following formula (I): R1-R2-N(R3)-R4-R5, where R1 represents non-substituted phenyl group; R2 represents hydrocarbon chain, containing 0-4 carbon atoms, preferably 1-4 carbon atoms; R3 represents hydrocarbon chain, containing 1-3 carbon atoms; R4 represents hydrocarbon chain, containing 1-5 carbon atoms; and R5 represents OH or H. As base matrix contains particles, in fact representing spherical particles, or has membranous or porous structure. Method of obtaining separation matrix includes immobilisation of said ligand on base mainly through amine group. Obtained matrix is placed into chromatographic column and after that sterilised if necessary. In order to separate one or more antibodies from one or more other compounds in liquid sample mobile phase, containing said antibodies and compound(s), are brought into contact with separation matrix. Liquid sample can contain supernatant, obtained in cell fermentation or unprocessed nutritional substance. In the process of application of chromatographic column mobile phase passes through column under impact of gravity and/or rocking, and antibodies are obtained in flow liquid of column. Invention also described set for purification of antibodies from one or more other components in liquid, containing in separate compartments chromatographic column, filled with separation matrix, one or more than one buffer and written instructions.
EFFECT: claimed invention relates to novel separation matrix, containing ligand, bound to base.
20 cl, 6 dwg, 4 tbl, 4 ex
FIELD: process engineering.
SUBSTANCE: proposed invention relates to method of fabricating of additive for hydraulic processing. Said process comprises the steps that follow. Carbon-bearing stock is fed to primary grinding zone to obtain ground material with particle size smaller than that of carbon-bearing stock. Ground material is dried to get moisture content smaller than about 5 wt %. Said dry ground material is fed to distribution zone to separate the particles of required size from those of inadequate size. Particle of required size are heated to 300-1000°C. Heated particles are cooled to magnitude smaller that about 80°C to get the additive. Target additive comprises solid organic material with particle size of 0.1-2000 mcm, bulk density varies from 500 to about 2000 kg/m3, structural density of 1000 to about 2000 kg/m3 and moisture content of about 0-5 wt %. Besides, this invention relates to hydraulic processing process. At application of additive in compliance with this invention, hydraulic processing can be effected at high transformation degree.
EFFECT: higher efficiency.
25 cl, 4 ex, 10 tbl, 6 dwg
SUBSTANCE: ganglia of cephalopods are homogenised by double sonication. The obtained homogenate is diluted with distilled water, the mixture is filtered, centrifuged and the supernatant is passed through a chromatography column, where the sorbent is used as concanavalin A-sepharose (Con-A-sepharose), and dried, and prior to drying the propionylcholinesterase the solution of polyethylene glycol is added to the enzyme solution. The enzyme solution is sublimated at a temperature of final drying not exceeding 30°C.
EFFECT: obtaining propionylcholinesterase with optimal specific activity on industrial scale.
2 cl, 1 ex
SUBSTANCE: invention relates to an improved chromatographic fractionation method for purification of polyunsaturated fatty acids and derivatives thereof. The method for chromatographic separation of a product - polyunsaturated fatty acid - from a starting mixture includes feeding the starting mixture into a simulated or true moving bed chromatographic apparatus, having a plurality of connected chromatographic columns containing aqueous alcohol as an eluent, where the apparatus has a plurality of areas which include at least a first area and a second area, each area having an extract stream and a raffinate stream, from which liquid can be collected from said plurality of connected chromatographic columns, and where (a) the raffinate stream, containing the polyunsaturated fatty acid product along with more polar components, is collected from a column in the first area and is fed into a non-adjacent column in the second area and/or (b) the extract stream, containing the polyunsaturated fatty acid product along with less polar components, is collected from a column in the second area and fed into a non-adjacent column in the first area, wherein said polyunsaturated fatty acid product is separated from the other components of the starting mixture in each area.
EFFECT: method provides efficient separation of polyunsaturated fatty acids or derivatives thereof from more polar and less polar impurities to obtain substantially pure polyunsaturated fatty acids and derivatives thereof.
16 cl, 15 dwg, 4 tbl, 9 ex
SUBSTANCE: natural zeolite clinoptilolite is activated in pulse magnetic field with value of magnetic induction 11 mT and activation time 0.5 min and introduced into polluted with petrol water.
EFFECT: invention makes it possible to increase degree of sewage water pollution from petrol, reduce energy consumption and realise environment friendly purification process.
SUBSTANCE: one of the method versions includes: bringing a hydrocarbon flow in contact with, at least, one sorbent, which adsorbs, at least, a part of admixtures from the hydrocarbon flow with obtaining a purified hydrocarbon flow; after that, separation of the purified hydrocarbon flow from, at least, one sorbent; then, preliminary processing of, at least, one sorbent before the stage of contact, where the stage of preliminary processing represents manufacturing a sorbent, capable of adsorbing admixtures; where the stage of preliminary preparation includes: a) washing the sorbent with a solvent, b) regulation of pH of the sorbent, present in the solvent to pH higher than 10, c) deaeration of the sorbent, present in the solvent, d) removal of the solvent from the sorbent and e) the sorbent drying. The sorbent represents clay.
EFFECT: application of the claimed invention makes it possible to obtain monomers with an increased stability, prevent the contamination of processing systems and provide more complete reproducibility of polymerisation reactions.
17 cl, 2 ex, 4 tbl, 1 dwg
SUBSTANCE: method includes the following stages: interaction of eluate 68Ge/68Ga generator with a cation-exchange resin, washing the cation-exchange resin with a mixture of hydrochloric acid and ethanol, eluting 68Ga from the cation-exchange resin with the mixture of hydrochloric acid and ethanol, interaction of the obtained eluate with an anion-exchange resin, washing the anion-exchange resin with ethyl alcohol, drying the anion-exchange resin with air or inert gas and eluting 68Ga from the anion-exchange resin with a water solution of hydrochloric acid.
EFFECT: increased output of the process.
2 tbl, 2 dwg, 3 ex
SUBSTANCE: invention relates to a method of adsorptive separation of one compound from a mixture of C8 aromatic hydrocarbons, namely from para-xylol. The method of separating para-xylol from the mixture of an initial raw material includes bringing liquid, which contains an undesirable isomer, in contact with a layer of adsorbent, which includes crystals of a metal-organic framework, selected from the group, consisting of Al-MIL-53, Zn-MOF-5 and their mixtures, and extraction of para-xylol from the adsorbent. The said crystals of the metal-organic framework adsorb para-xylol and make it possible for meta-xylol, ortho-xylol and ethylbenzene to pass through the said crystals of the metal-organic framework without adsorption.
EFFECT: method provides separation of para-xylol from other C8 aromatic hydrocarbons.
8 cl, 9 dwg, 5 tbl, 2 ex
SUBSTANCE: means represents a dry extract of leaves and flowers of Gratiola officinalis, obtained by milling the leaves and flowers of Gratiola officinalis, extraction with 96% alcohol on a water bath to boiling and boiling, evaporation, dilution of the evaporated residue first with distilled water, then by the addition of chloroform, cooling to room temperature and centrifuging with the following separation of a water fraction and drying it under specified conditions.
EFFECT: means is non-toxic, has an expressed anti-tuberculosis action.
2 tbl, 2 ex
SUBSTANCE: method of producing α(1,2)-L-skeleton-α(1,4)-D-galactopyranosyluronan from Acorus calamus L rhizome is carried out in two steps. At the first step, crushed material is extracted with acidified water and heated on a boiling water bath while periodically mixing; after settling, the mixture is heated once more, left to cool to room temperature and filtered through a multilayer fabric filter; the filtrate is evaporated under a vacuum; the obtained solution is slowly added to 96% ethyl alcohol or to a solution of reclaimed ethanol and left in a cool place to settle the residue, after which the settled solution is drained, and the residue is filtered through a paper filter by successively washing with 96% ethyl alcohol and then with acetone. At the second step, without drying, the residue is transferred from the filter and dissolved in purified water while stirring rapidly; the obtained solution is then centrifuged; the obtained solution is purified from low-molecular weight compounds by filtering through a semi-permeable membrane; the purified solution is frozen and freeze-dried at certain conditions.
EFFECT: improved method.
3 dwg, 6 tbl
SUBSTANCE: method for producing Befungin, a preparation of Chaga mushroom involving extracting the milled raw material in heated water on a heating unit consisting of 3 reactors; adding cobalt salts to the extract in certain environment, mixing with ethanol, evaporating to dry residue of 20-25%.
EFFECT: method enables accelerating the production process, reducing energy demands, improving the quality and completeness of extraction, and improving the quality of the preparation.
2 dwg, 1 tbl, 1 ex
SUBSTANCE: invention represents the method to obtain the soluble concentrate from sideline products of reindeer antlers, comprising aqueous raw extraction, grounded up to the forced meat condition with particle size of 3-5 mm under the action of ultrasonic vibrations with frequency of 37 kHz with subsequent filtration and vacuum drying at temperature of 45°C and pressure of 0.9 atm, distinguished by the fact that the aqueous raw extraction is carried out at temperature of 35-36°C in the presence of pepsin ferment at its concentration in raw mixture: water of 0.5% during at least 3 hours, at ratio raw: water for tails 1:5, for male genital 1:4, for uteruses with embryos and amniotic fluid 1:2.
EFFECT: significant increase of final concentrate yield from sideline products of reindeer antlers.
3 ex, 2 tbl
SUBSTANCE: invention relates to method of simultaneous obtaining of two flavonoids - patuletine and its 7-O-β-D-glucopyranoside - patuletrine. Method consists in the following: milled edge petals of flower of high flavonoid sorts of tagetes patula are extracted with hexane, dried and r-extracted with chloroform, chloroform extract is concentrated, dry residue is dissolved in mixture of petroleum ether - chloroform, precipitated sediment is filtered, washed with petroleum ether and dried, obtained dry powder is dissolved in mixture chloroform - ethanol, precipitated sediment is filtered, washed with petroleum ether and dried with obtaining patuletine. Then, extraction of raw material, which remains after chloroform processing, is carried out with ethanol, alcohol extract is filtered and concentrated, after that, water residue is subjected to liquid phase extraction with ethylacetate, then, organic layer is concentrated, dry residue is dissolved in mixture chloroform - ethylacetate, precipitated sediment is filtered, washed with cooled ethylacetate, solution of hydrochloric acid in ethanol, ethanol and ethylacetate and dried, dry powder is dissolved in mixture ethylacetate-ethanol, precipitated sediment is filtered, washed with ethylacetate and dried with obtaining patuletrine.
EFFECT: method makes it possible to obtain highly pure samples of patuletine and patuletrine, as well as increase target product output.
4 dwg, 3 tbl, 4 ex
FIELD: medicine, pharmaceutics.
SUBSTANCE: invention refers to pharmaceutical industry, namely to a method for preparing lappaconitine hydrobromide (versions) A method for preparing lappaconitine hydrobromide is implemented by extraction of Aconitum leucostomum root and herb or Aconitum septentrionale root and herb in methylene chloride in a continuous extraction apparatus that is followed by decontamination by means of flash chromatography (version 1), or extraction of a herbal raw material in a polar organic solvent followed by extract removal from the organic solvent (version 2), alkalinisation and extraction of the prepared extract in methylene chloride followed by decontamination of the extract by flash chromatography.
EFFECT: method for preparing lappaconitine hydrobromide provides simplifying the technological process, reducing its length and improving higher yield of the end product of officinal purity.
7 cl, 1 tbl, 9 ex
FIELD: food industry.
SUBSTANCE: method for production of Siberian cedar seeds liqueur (with hepatoprotective, antioxidant, antihypoxic, hypolipidemic effect) by way of maceration with ethyl alcohol usage; whole Siberian cedar seeds are loaded into the reactor, poured with 70% ethyl alcohol water solution; extraction is performed under preset conditions. The medicinal preparation with hepatoprotective, antioxidant, antihypoxic, hypolipidemic effect contains Siberian cedar seeds liqueur. Usage of the medicinal preparation as a hepatoprotective remedy.
EFFECT: liqueur has pronounced hepatoprotective, antioxidant, antihypoxic and hypolipidemic effect.
6 cl, 3 dwg, 8 tbl
SUBSTANCE: method for producing a pigment complex of bisnaphthazarin for preventing inflammatory diseases, involving demineralising commercial sea urchins' crusts and needles in an organic acid solution, separating organic acid salts and protein, applying pigment solution on a chromatographic column, washing the column with diluted mineral acid and distilled water, eluting the pigment complex, combining fractions containing the pigments, removing ethanol, lyophilising concentrate in the certain environment. The complex of pigments bisnaphthazarins for preventing inflammatory diseases.
EFFECT: complex of pigments prepared by the above method is effective for preventing the inflammatory diseases.
3 cl, 2 dwg, 2 tbl, 4 ex
FIELD: machine building.
SUBSTANCE: for extraction (leaching) of the substances extracted from the plant materials in food, chemical-pharmaceutical and other industries, for output increasing of the substances extracted from the extractable plant materials and for increasing of their concentration in the ready extraction it is suggested to provide the extractor with the extractant recirculation circuit containing devices for solid phase separation, pump, discharge tank, flowmeter, shutdown valves system, and in the extractor bottom part additionally union will be installed for continuous liquid phase supply.
EFFECT: wider possibility of return in the vessel of part of extraction after solid phase separation in specified ratio with fresh extractant, thus improving conditions of mass exchange due to decreasing of the surface tension of the liquid phase.
SUBSTANCE: method for preparing an agent possessing anti-inflammatory, diuretic and antioxidant activity, involving milling Spiraea salicifolia shoots representing a mixture of leaves, blossom and shoots, extracting them three times by gradual maceration, mixing in infusing, filtering, condensing, separating, drying in the certain environment.
EFFECT: agent shoes the pronounced anti-inflammatory, diuretic and antioxidant activity.
2 dwg, 12 tbl
SUBSTANCE: invention relates to medicine, in particular to application of medication "Osteomed" for treating arthritis and arthrosis.
EFFECT: said application makes it possible to accelerate treatment of arthritis and arthrosis, increased efficiency of such treatment with simultaneous elimination of risk of hypercalcemic condition development.