WO2009031934A1 - Method for producing vegetable cell sap concentrate and means for the production thereof - Google Patents
Method for producing vegetable cell sap concentrate and means for the production thereof Download PDFInfo
- Publication number
- WO2009031934A1 WO2009031934A1 PCT/RU2008/000483 RU2008000483W WO2009031934A1 WO 2009031934 A1 WO2009031934 A1 WO 2009031934A1 RU 2008000483 W RU2008000483 W RU 2008000483W WO 2009031934 A1 WO2009031934 A1 WO 2009031934A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- carbon dioxide
- liquefied carbon
- extraction
- water
- liquefied
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Definitions
- the invention relates to the extraction of biologically active substances from plant materials and is based on the use of liquefied carbon dioxide.
- the invention can be used in the pharmaceutical, perfumery, cosmetic and food industries.
- the claimed group of inventions is intended to create an aqueous fraction of plants, which is an almost natural concentrated cell sap extracted from a freshly picked plant using liquefied carbon dioxide.
- the concept of “cell juice” is used [1].
- cell sap is a fluid secreted by the cytoplasm of a living plant cell, filling its vacuoles.
- the vacuole contains cellular juice, which is water with mineral and organic substances dissolved in it.
- Cellular juice is specific for the family and even for the species of plants, depending on the growing conditions, age of the plant and its individual cells.
- the accumulation of cellular juice inside the protoplasm is a purely physical process that can be produced artificially.
- the methods for their preparation are based, for example, on steam distillation of biologically active substances [2], extraction of plant materials using an organic solvent and diluting the obtained extract with water [3], or a water-ethanol mixture [4], extracting plant materials under pressure in two stages [5].
- an aqueous extract of fir is obtained by treating the raw materials with hot steam for 1.5-2 hours, the resulting vapor-gas mixture is removed and the aqueous extract is separated from the oil.
- liquefied carbon dioxide as an extractant is known in the art. So in the method of extraction of plant materials with liquefied gases [5], the extraction of plant materials is carried out under pressure in two stages, while flow extraction is carried out at a pressure exceeding the filling pressure, and the pressure between stages is released to the filling pressure.
- the conditions of the method provide effective impregnation of raw materials, which helps to increase the degree of extraction of the necessary components from the deep layers of the raw material in a shorter period of time.
- carotenoids, chlorophyll compounds and other necessary components for example, a lipid fraction
- target biologically active components for example, a lipid fraction
- the closest in technical essence and the achieved result is a method of processing the bark of coniferous trees [7], including grinding, moistening and extraction with liquefied carbon dioxide, at elevated pressure and room temperature, separation of the carbon dioxide extract into oily and aqueous fractions, while the aqueous fraction is extracted with chloroform .
- liquefied carbon dioxide is not used to obtain cell juice in its native form, but is used to extract water, which at the beginning of the processing process is used to moisten the bark and dissolve the maltol extracted from the bark of conifers.
- the objective of the invention is to obtain concentrated cell juice using as a means for its production of liquefied carbon dioxide.
- the technical result is the provision of the possibility of obtaining concentrated cell juice. At the same time, the yield and quality of useful substances of plant raw materials are increased due to the production of concentrated cellular juice in its native form.
- the problem is solved in that in the known method, including the extraction of crushed raw materials liquefied carbon dioxide at room temperature and the separation of the oil fraction, extraction is carried out with a large flow of liquefied carbon dioxide based on the proportion of not less than 1 liter of carbon dioxide per 1 g of plant cell juice extraction, and concentrated cell juice is obtained by separating the oil fraction from the aqueous fraction.
- the technical result is achieved mainly due to the fact that liquefied carbon dioxide is used as a means to obtain concentrated plant cell juice. It is preferable to carry out the extraction of the raw materials with liquefied carbon dioxide in the extractor by feeding the liquefied carbon dioxide from the storage device installed at a height of at least 8-12 m above the extractor.
- the extraction of raw materials with liquefied carbon dioxide can also be carried out by supplying liquefied carbon dioxide with a metering pump.
- Extraction with liquefied carbon dioxide provides selective and fairly complete separation of cell juice in the form of an aqueous fraction from plant materials, since liquid carbon dioxide dissolves both water and water-soluble compounds. This is because the solubility of water in liquid carbon dioxide is 0.1%, i.e. in order to obtain 1 kg (or liter) of cell juice at the outlet, it is necessary to pass 1000 kg of liquid carbon dioxide through plant material. To isolate the oil fraction in an amount of 1 kg, several tens of liters of liquid carbon dioxide are sufficient. Therefore, to isolate cell juice in the form of an aqueous fraction, it is necessary to skip a sufficiently large amount in a flow extractor liquid carbon dioxide.
- the installation height of the liquid carbon dioxide accumulator above the extractor is 0.5 - 1 m. Therefore, the extractant duct is sufficient to isolate the oil fraction, but insufficient to isolate the aqueous fraction.
- the flow of carbon dioxide can be achieved due to the height of the liquid column. Structurally, this is achieved by creating a differential pressure by raising the storage of liquefied carbon dioxide to a height of 8-12 m above the extractor. This problem can also be solved by using a high pressure pump.
- the extraction process occurs at room temperature, which does not lead to destructive changes in chemical compounds, and the cell juice extracted from freshly picked plant materials using liquefied carbon dioxide under pressure is presented in its native form without temperature treatment.
- the aqueous extract is a natural cellular juice of a plant subjected to extraction, containing a whole complex of biologically active substances.
- liquefied carbon dioxide for the extraction process is known, however, its use as a means to obtain concentrated cell juice in the prior art was not found. It is generally recognized that extraction from plant materials with the help of liquefied carbon dioxide of essential oils and other fat-soluble plant components. However, in liquefied carbon dioxide, water and water-soluble substances of plants are dissolved in a small amount, water (0.1%) - At the end of the extraction process and removal of carbon dioxide By depressurization, water and water-soluble substances are rejected by the oil fraction and released into a separate phase.
- a method of isolating an aqueous extract of fir is as follows.
- the crushed plant mass preferably freshly harvested, is exhaustively extracted with liquefied carbon dioxide at room temperature and a pressure of 64 ⁇ 6 atm (a sufficient extraction time of 3 hours) in a flow extractor with an increased flow of liquid carbon dioxide by raising the liquid carbon dioxide accumulator above the extractor to a height of 8-12 meters.
- the increase in the flow of liquid carbon dioxide through the extracted plant material is ensured by increasing the column of liquid carbon dioxide above the extractor, as a result of which the pressure of the column of liquid on the feed increases proportionally.
- An increase in the flow of liquid carbon dioxide through extractable plant materials can also be achieved through the use of a metering pump.
- carbon dioxide is removed from it and a total extract is obtained, which, when standing or centrifuging, is divided into two fractions - oil and water.
- the output of the aqueous fraction of the carbon dioxide extract of the plant is a cell sap with a high concentration of biologically active substances.
- Using the proposed method allows to obtain an extract of water-soluble compounds of plants - cell juice without reducing their biological activity. This is because the carbon dioxide extraction of plant materials does not lead to any destructive changes in organic molecules, because the process occurs at room temperature, and carbon dioxide is universally considered an inert gas.
- the concentration of cell juice using the applied liquefied carbon dioxide is explained by the following. Let us consider the process of concentration of intracellular juice during carbon dioxide extraction using the example of a fir foot, as the most commonly used raw material for the production of carbon dioxide extract of fir. These considerations apply to any other plant. About 1000 kg of water are contained in 1000 kg of a freshly picked fir foot (humidity of a freshly picked fir foot is 55–65%). Experimental data showed that the specified raw materials of water-soluble biologically active components, namely, ascorbic acid, maltol, organic salts, etc. contain only about 0.6 kg. If hypothetically suggest that there was a complete extraction of these compounds together with water, then we get the intracellular juice of the plant (600 kg with a dry residue of OD%).
- the process of carbon dioxide extraction is independent or weakly correlated with temperature and pressure.
- the pressure above liquid carbon dioxide uniquely depends on temperature, i.e. as the temperature rises, so does the pressure.
- Room temperature which is usually in the range of 15-30 C, corresponds to a pressure of 40-74 atm.
- Example 1 Freshly harvested and chopped wood greens of Siberian fir (58 kg) are subjected to steam distillation at a temperature of 100 - 180 0 C and a pressure of 1 -2 atm for 10-24 hours.
- the yield of essential oil is 1.45 kg (2.5 % by weight of the original woody green).
- the output of the aqueous fraction is 45 kg.
- the aqueous fraction contains 0.009% solids.
- Example 2 Dried and crushed to particles of not more than 5 mm wood greens of Siberian fir (58 kg) are extracted in a flow extractor with a liquid column height of 0.5 m liquefied carbon dioxide at a temperature of 20 0 C and a pressure of 64 atm for 3 hours. Yield 1.8 kg (3.1% by weight of the initial woody green). There is no water fraction.
- Example 3 Freshly harvested and chopped wood greens of Siberian fir (58 kg) are extracted in a conventional flow extractor with liquefied carbon dioxide at a temperature of 20 0 C and a pressure of 64 atm for 3 hours. Yield 1.2 kg (2, l% of the initial mass wood greens) oil fraction. An aqueous fraction of 80 g gives an emulsion with an oil fraction, is considered defective and, after prolonged settling or centrifugation, is usually discarded as a wet, solid product used to isolate maltol. The amount of water was determined by the gravimetric method when the wet, solid “small powder” was dried. According to the calculation, the total flow of liquefied carbon dioxide is 80 liters. Example 4.
- Freshly harvested and chopped wood greens of Siberian fir (58 kg) are extracted in a flow extractor with liquefied carbon dioxide with a large flow of liquefied carbon dioxide by raising the accumulator of liquefied carbon dioxide to a height of 10 m above the extractor at a temperature of 20 0 C and a pressure of 64 atm for 3 hours.
- the yield of the total extract is 2.3 kg (4.0% by weight of the initial woody greens). After settling or centrifugation, two fractions are obtained - oil 1.4 kg (4%) and aqueous 0.9 kg (1.6%). According to the calculation, the total flow of liquefied carbon dioxide was 900 liters.
- the product obtained in example 4 has the form of a dark red solution, soluble in water, alcohol.
- the content of ascorbic acid is 750 mg / kg.
- Example 5 Freshly harvested and chopped wood greens of Siberian fir (58 kg) are extracted in a flow extractor with liquefied carbon dioxide with a large flow of liquefied carbon dioxide by raising the accumulator of liquefied carbon dioxide to a height of 8 m above the extractor at a temperature of 20 0 C and a pressure of 64 atm within 3 hours.
- the yield of the total extract is 2, 1 kg (3.6% by weight of the initial woody greens). After settling or centrifugation, two fractions are obtained - oil 1.4 kg (2.4%) and water 0.7 kg (1.6%). According to the calculation, the total flow of liquefied carbon dioxide was 700 liters.
- Example 6 Freshly harvested and chopped wood greens of Siberian fir (58 kg) are extracted in a flow extractor with liquefied carbon dioxide with a large flow of liquefied carbon dioxide by raising the storage of liquefied carbon dioxide to a height of 12 m above the extractor at a temperature of 20 0 C and a pressure of 64 atm within 3 hours.
- the yield of the total extract is 2.5 kg (4.3% by weight of the initial woody greens).
- two fractions are obtained - oil 1.4 kg (2.4%) and aqueous 1.1 kg (1.9%). According to the calculation, the total flow of liquefied carbon dioxide was 1100 liters.
- Example 7 Freshly picked greens of a birch leaf in an amount of 2.7 kg are treated as in Example 4. The yield of the total extract is 52 g. After centrifugation, two fractions are obtained - 21 g oil and 3 g water.
- Example 8 Freshly collected nettle greens in an amount of 9.2 kg is treated as in Example 4. The yield of the total extract is 802 g. After centrifugation, two fractions are obtained - oil fraction 482 g and aqueous 320 g.
- Example 9 Freshly picked green leaves of lingonberry in an amount of 6.7 kg are treated as in example 4. The yield of the total extract is 680 g. After centrifugation, two fractions are obtained - oil fraction 8 g and aqueous 672 g.
- Example 10 Freshly picked green leaf of currant in an amount of 8.2 kg is treated as in example 4. The yield of the total extract is 97 g. After centrifugation, two fractions are obtained - oil fraction 74 g and aqueous 23 g.
- Example 11 The pulp of sea buckthorn berries in an amount of 9.7 kg is processed as in example 4. The yield of the total extract is 286 g. After centrifugation, two fractions are obtained - oil 3 g and water 283 g.
- Example 12 The pulp of viburnum berries in the amount of 6.87 kg is processed as in example 4. The yield of the total extract is 135 g. After centrifugation, two fractions are obtained - oil fraction 92 g and aqueous 42 g.
- Example 13 Freshly harvested and chopped wood greens of Siberian fir (58 kg) are extracted in a flow extractor with liquefied carbon dioxide with a large flow of liquefied carbon dioxide through the use of a high-pressure liquid pump with a set flow rate of 100 l / h at a temperature of 20 0 C and a pressure of 64 atm for 3 hours.
- the total extract yield is 1.7 kg (2.9% by weight of the initial woody green).
- two fractions are obtained - oil 1.4 kg (4%) and aqueous 0.3 kg (0.5%). According to the calculation, the total flow of liquefied carbon dioxide was 300 liters.
- Example 13 The product obtained in example 13, has the form of a dark red solution, soluble in water, alcohol. The dry residue is 3.0%.
- Example 14 Freshly collected and crushed to particles no more than
- the product obtained in example 14 has the form of a dark red solution, soluble in water, alcohol.
- the dry residue is 2.9%.
- liquefied carbon dioxide made it possible to obtain an aqueous fraction of plants, which are intracellular water of the plant itself with biologically active substances dissolved in it in a concentrated form, i.e. concentrated cell juice.
- cell sap contains useful natural substances in native (live) form in a maximum, concentrated amount.
- the claimed invention can be used in the pharmaceutical, perfumery, cosmetic and food industries.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Botany (AREA)
- Animal Behavior & Ethology (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Biotechnology (AREA)
- Wood Science & Technology (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- General Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Alternative & Traditional Medicine (AREA)
- Epidemiology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
- Cosmetics (AREA)
- Non-Alcoholic Beverages (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Claims
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP08794081.3A EP2186522B1 (de) | 2007-08-07 | 2008-07-22 | Verfahren zur herstellung eines pflanzlichen zellsaftkonzentrats |
| AU2008295631A AU2008295631B2 (en) | 2007-08-07 | 2008-07-22 | Method for producing vegetable cell sap concentrate and means for the production thereof |
| US12/700,946 US9173911B2 (en) | 2007-08-07 | 2010-02-05 | Method for producing vegetable cell sap concentrate and means for the production thereof |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2007130259/15A RU2358746C2 (ru) | 2007-08-07 | 2007-08-07 | Способ получения концентрированного клеточного сока и средство для его получения |
| RU2007130259 | 2007-08-07 |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US12/700,946 Continuation US9173911B2 (en) | 2007-08-07 | 2010-02-05 | Method for producing vegetable cell sap concentrate and means for the production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2009031934A1 true WO2009031934A1 (en) | 2009-03-12 |
Family
ID=40429106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/RU2008/000483 Ceased WO2009031934A1 (en) | 2007-08-07 | 2008-07-22 | Method for producing vegetable cell sap concentrate and means for the production thereof |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US9173911B2 (ru) |
| EP (1) | EP2186522B1 (ru) |
| AU (1) | AU2008295631B2 (ru) |
| MY (1) | MY149377A (ru) |
| RU (1) | RU2358746C2 (ru) |
| WO (1) | WO2009031934A1 (ru) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2523038C2 (ru) * | 2011-05-12 | 2014-07-20 | Учреждение Российской академии наук Институт фундаментальных проблем биологии Российской академии наук (ИФПБ РАН) | Способ выделения билогически активных компонентов из растительного сырья и средство на его основе |
| RU2673905C1 (ru) * | 2017-12-01 | 2018-12-03 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Новосибирский государственный аграрный университет" | Способ приготовления варенья |
| RU2701562C1 (ru) * | 2018-04-05 | 2019-09-30 | Вилави Инт Лтд | Композиция на основе хвойной зелени и способ её получения |
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| RU2061491C1 (ru) | 1993-02-04 | 1996-06-10 | Николай Яковлевич Костеша | Способ получения средства, повышающего резистентность организма |
| RU2067977C1 (ru) | 1993-09-17 | 1996-10-20 | Красноярская государственная технологическая академия | Способ переработки коры хвойных деревьев |
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| JP3155003B2 (ja) * | 1990-11-06 | 2001-04-09 | サントリー株式会社 | ホップエキスの製造法および該方法により得られるホップエキス |
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2007
- 2007-08-07 RU RU2007130259/15A patent/RU2358746C2/ru active
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2008
- 2008-07-22 WO PCT/RU2008/000483 patent/WO2009031934A1/ru not_active Ceased
- 2008-07-22 MY MYPI2010000578A patent/MY149377A/en unknown
- 2008-07-22 AU AU2008295631A patent/AU2008295631B2/en not_active Ceased
- 2008-07-22 EP EP08794081.3A patent/EP2186522B1/de not_active Not-in-force
-
2010
- 2010-02-05 US US12/700,946 patent/US9173911B2/en active Active
Patent Citations (9)
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| SU1346111A1 (ru) * | 1985-07-12 | 1987-10-23 | Грузинский Институт Субтропического Хозяйства | Способ производства концентрата ча |
| RU2061491C1 (ru) | 1993-02-04 | 1996-06-10 | Николай Яковлевич Костеша | Способ получения средства, повышающего резистентность организма |
| RU2039586C1 (ru) | 1993-07-07 | 1995-07-20 | Акционерное общество закрытого типа "Алтайвитамины" | Способ экстракции растительного сырья сжижженными газами |
| RU2067977C1 (ru) | 1993-09-17 | 1996-10-20 | Красноярская государственная технологическая академия | Способ переработки коры хвойных деревьев |
| RU2125459C1 (ru) | 1997-06-10 | 1999-01-27 | Закрытое акционерное общество "Алтайвитамины" | Способ получения биологически активных веществ из облепихового сырья |
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Also Published As
| Publication number | Publication date |
|---|---|
| US9173911B2 (en) | 2015-11-03 |
| EP2186522A4 (de) | 2011-01-12 |
| US20100136149A1 (en) | 2010-06-03 |
| RU2358746C2 (ru) | 2009-06-20 |
| AU2008295631B2 (en) | 2012-02-02 |
| AU2008295631A1 (en) | 2009-03-12 |
| RU2007130259A (ru) | 2009-02-20 |
| MY149377A (en) | 2013-08-30 |
| EP2186522B1 (de) | 2018-01-24 |
| EP2186522A1 (de) | 2010-05-19 |
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