WO2016118034A2 - Process and installation for extraction of biological active compounds from plants and continuous reactor for ultrasound and microwave assisted extraction of biological active compounds from plants - Google Patents
Process and installation for extraction of biological active compounds from plants and continuous reactor for ultrasound and microwave assisted extraction of biological active compounds from plants Download PDFInfo
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- WO2016118034A2 WO2016118034A2 PCT/RO2016/050001 RO2016050001W WO2016118034A2 WO 2016118034 A2 WO2016118034 A2 WO 2016118034A2 RO 2016050001 W RO2016050001 W RO 2016050001W WO 2016118034 A2 WO2016118034 A2 WO 2016118034A2
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- Prior art keywords
- extraction
- mixture
- solvent
- active biological
- microwaves
- Prior art date
Links
- 238000000605 extraction Methods 0.000 title claims abstract description 115
- 150000001875 compounds Chemical class 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000009434 installation Methods 0.000 title claims abstract description 7
- 238000000874 microwave-assisted extraction Methods 0.000 title description 2
- 238000002137 ultrasound extraction Methods 0.000 title 1
- 239000000203 mixture Substances 0.000 claims abstract description 52
- 238000002604 ultrasonography Methods 0.000 claims abstract description 30
- 239000000341 volatile oil Substances 0.000 claims abstract description 20
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 11
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 11
- 235000010208 anthocyanin Nutrition 0.000 claims abstract description 9
- 229930002877 anthocyanin Natural products 0.000 claims abstract description 9
- 239000004410 anthocyanin Substances 0.000 claims abstract description 9
- 150000004636 anthocyanins Chemical class 0.000 claims abstract description 9
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 9
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 9
- 239000010685 fatty oil Substances 0.000 claims abstract description 6
- 235000007586 terpenes Nutrition 0.000 claims abstract description 6
- 150000003505 terpenes Chemical class 0.000 claims abstract description 5
- 229930004725 sesquiterpene Natural products 0.000 claims abstract description 3
- -1 sesquiterpenes compounds Chemical class 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 39
- 239000002904 solvent Substances 0.000 claims description 36
- 238000003860 storage Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 241000196324 Embryophyta Species 0.000 description 43
- 239000012620 biological material Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000005445 natural material Substances 0.000 description 9
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 235000018102 proteins Nutrition 0.000 description 5
- 244000178231 Rosmarinus officinalis Species 0.000 description 4
- 239000006286 aqueous extract Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- 240000007049 Juglans regia Species 0.000 description 2
- 235000009496 Juglans regia Nutrition 0.000 description 2
- 235000001466 Ribes nigrum Nutrition 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 241000857902 Bursera graveolens Species 0.000 description 1
- 240000001890 Ribes hudsonianum Species 0.000 description 1
- 235000016954 Ribes hudsonianum Nutrition 0.000 description 1
- 241001312569 Ribes nigrum Species 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 240000004978 Rosa x damascena Species 0.000 description 1
- 235000011402 Rosa x damascena Nutrition 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000007797 non-conventional method Methods 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 235000015639 rosmarinus officinalis Nutrition 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 235000017709 saponins Nutrition 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- 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
- B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Definitions
- the present invention refers to a process for extraction of active biological compounds from plants by simultaneous application of ultrasounds and microwaves and a new type, continuous, chemical reactor for extraction of active biological compounds from plants provided with means for simultaneous application of ultrasounds and microwaves.
- invention refers to an installation for continuous extraction of active biological compounds from plants with the new type of chemical reactor for extraction.
- Patent application EP 1439218 A1 describes extraction processes of volatile oils from different types of plant materials and microwaves assisted devices for the related processes as described.
- Patent application EP 1439218 A1 describes an extraction process of natural volatile substances from biological materials by hydrodistillation by means of microwaves, without addition of solvent.
- the patent application EP 1439218 A1 refers to a microwave extraction apparatus of volatile compounds from biological material by a hydrodistillation process, which comprises a microwave oven, with a microwave chamber for receiving the biological material and a condensation chamber wherein, the condensation chamber is situated above the microwave chamber and is connected to the microwave chamber through a channel bundle.
- This system improves the condensation and cooling area of the water vapours from outside of the microwave chamber.
- this extraction process takes place with relatively low yields and the extraction apparatus has a functioning in batch system, applicable for small quantities of biological material.
- Another extraction method of the volatile oils from biological material consists of microwave application to biological material under low pressure conditions until the natural substances are released from the biological material and followed by their condensation, as described in patent application EP 1618798 A1. Further, the application EP 1618798 A1 describes an apparatus with the following components: a microwave cavity with a receiving region of the microwaves, allowing a low pressure in microwave area and a condensation chamber, which are connected by a tube.
- Another extraction method of the volatile substances which have a low solubility in water, from biological material is described in the patent EP 1629725 B1.
- the extraction method as presented in patent includes the following steps:
- the water carrying natural substances partially returns in the microwave area by a drainage system.
- the natural substances or the least soluble in water are separated from the hydrophobic solvent.
- the water vapours are generated inside the microwave cavity from the mixture water/biological material.
- Disclosure of invention The technical problem solved by the present invention is given by the need to get a higher yield of extraction, with high purity of the extraction product, and to obtain also other valuable components such as polyphenols, anthocyanins, proteins, etc, whilst processing a much higher quantity of biological material.
- a first object of the invention is a process for extraction of active biological compounds from plants which comprises the following steps:
- the mixture of plant material and solvent released from extraction zone is reintroduced in the extraction zone, recirculating so until all active biological compounds are extracted. Then, the liquid extraction mixture is separated from the plant material and is processed for obtaining the active biological compounds.
- Another object of invention is a continuous reactor for extraction of active biological compounds, in the form of a pipeline, whose length is substantially higher than the diameter thereof and which assures a zone of extraction with a continuous flow regime, controlled, with supplying at one end and evacuation at the other end and which is provided with means for generating and simultaneous application of ultrasounds and microwaves and means for collecting the active biological compounds released in the extraction process.
- the reactor is provided with means for controlling and monitoring the temperature and working pressure, and the vacuum, the reflected and incident microwaves power as well as means for carrying out the extraction process under inert atmosphere, whenever this is necessary.
- the reactor diameter is between 10mm and 2200 mm, depending of the operating manner, production capacity and the type of plant material which is subjected to the extraction process.
- Another object of invention is an installation for extraction of active biological compounds from plants which comprises a continuous extraction reactor according to the present invention, connected to a circuit for the transportation of the mixture of plant material and solvent, which makes the connection from a storage vessel for the said mixture to the supplying end of the extraction reactor, and respectively, from the evacuation end of the extraction reactor, to the collecting vessel for the mixture and a pump for supplying the mixture in the extraction reactor.
- the process according to the invention has many advantages: the quantity of biological material processed per charge is at least 100 times higher than in the batch system, the foaming phenomenon of the biological material is avoided and implicitly the undesired events, the extraction yield of natural substances increases by at least minimum 25%, the time of extraction is significantly reduced, it is obtained a product of high purity and high quality in terms of chemical composition compared to other methods and systems for extraction in a field of microwave and/or non- conventional methods, such as: extraction under pulsed electrical field, enzyme- assisted extraction, extraction with liquids under pressure, extraction with supercritical fluids.
- the biological material subject to the extraction can be processed at the same time also for other valuable components, such as: polyphenols, anthocyanins, proteins, etc. Also, the process according to the invention presents the advantages:
- Figure 1 represents schematically an embodiment of an installation of extraction of active biological compounds with the recirculation of the mixture of plant material and solvent to be extracted according to the invention
- a continuous extraction reactor provided with means of generating and application of ultrasounds and microwaves and a system for collecting and condensing of active biological compounds resulted from the extraction process, connected to a transportation circuit for the plant material to be processed that makes the connection from a vessel for the said mixture to the supplying end of the extraction reactor, and respectively, from the evacuation end of the extraction reactor, back, to the vessel for the mixture and a process pump for supplying and recirculation.
- the plant material may be in the form of plants, seeds, fruits, flowers, wooden material.
- the plant material is milled at a grain size which must not be greater than 20 pm or chopped if the plant material subjected to extraction is fresh.
- the plant material may be fresh or dried.
- a storage vessel it is prepared a mixture of plant material with solvent and it is homogenized so that the whole quantity of plant material, respectively plant, wood or seeds to be in contact with the solvent.
- the mixing ratio, by weight, of plant material and solvent is dependent on the plant material to be extracted, shape, size, condition, and it is between 1 :2 and 1 :20, preferably between 1 : 2 and 1:10.
- the solvent may be polar or non-polar. Solvents used for extraction are chosen depending on the active biological compound pursued to be extracted.
- deionized water is suitable for extraction of essential oils, anthocyanins, tannins, saponins, terpenes, sesquiterpene.
- Ethanol is a solvent suitable for extraction, for example, of alkaloids, terpenes, tannins, polyphenols, flavonoids.
- Soybean oil, olive oil, coconut oil are suitable for extraction of fatty oils, terpene compounds, stabilized proteins.
- the mixture of plant material and solvent is supplied to a continuous extraction reactor by means of a process pump.
- the reactor is provided with means for the application of ultrasounds, in the form of a sonotrod (US) and means for the application of microwaves, in the form of a multi- mode or mono-mode microwave cavity (MW).
- US sonotrod
- MW mono-mode microwave cavity
- the reactor is provided with means for controlling and monitoring temperature and the working pressure, and vacuum, reflected and incident microwave power as well as means for ensuring carrying out the extraction process in an inert atmosphere, whenever this is necessary.
- the reactor is connected to a drive system with steam of Clevenger type or Florentine flask for the collection and separation of volatile oil.
- the ultrasounds and microwaves sources are turned on.
- the operational parameters are adjusted: time, temperature, vacuum level (where applicable), optionally, inert atmosphere, power of the ultrasounds, the incident power of microwaves, pump flow rate.
- the work flow rate is correlated with the power of microwaves and ultrasounds applied to the mixture of plant material and solvent, namely: the greater flow rate it is the higher power of microwaves and ultrasounds are.
- this proportion may be modified depending on the physical-chemical characteristics of the plant and/or the solvent and the rheqjogical characteristics of the mixture of plant material and solvent.
- the mixture of plant material and solvent is subjected to simultaneous irradiation of ultrasounds and microwaves.
- Power of ultrasounds sources is comprised between 100-1000 W/l and power of microwaves sources is comprised between 100-6000 W/l at a microwave frequency of 2450 MHz or GHz 914.
- the mixture of plant material and solvent is simultaneously irradiated with ultrasounds and microwaves, ultrasonic power ranging between 100-500 W/l and microwave powers between 200- 000 W/l and a frequency of 2450 MHz, at an extraction temperature in the range of 40 to 110 °C, at normal pressure, the extraction time of 10-120 min and a flow rate of the pump of 0.1 to 2 l/min.
- the extraction of active biological compounds is accomplished under required technological conditions. Depending on the nature of active biological product obtained, namely: essential oil, blend of polyphenols, anthocyanins, or proteins, they are cooled at room temperature, they are conditioned by filtration, drying, centrifugation or lyophilization and they are stored.
- various active biological compounds comprising for example: essential oils, fatty oils, blends of polyphenols, mixtures of anthocyanins, terpenes, sequiterpenes compounds, stabilized proteins or in pure form.
- the mixture is homogenized with a mechanical homogenizer for 30 min., at room temperature, at a speed of 50 rpm.
- the pump suction hose is inserted in the storage vessel, the pump is cpupled in order to supply with the continuous reactor, and is turned on at a flow rate of 1 L/min.
- the ultrasounds sources are turned on at a power of 200 W/L and microwaves at a power of 400 W/L, the Clevenger system of collecting the volatile oil is coupled and the extraction time is set at 90 minutes. After 90 minutes the extraction of the vp!gtile oil has been completed.
- the volatile oil is separate ⁇ from wafer apd jt is drj£d pn th anhydrous Na2S0 4 .
- the volatile oil thus obtained is stored in dark colour pots, at premises protected from light and heat.
- the extraction yield was calculated according to the Romanian Pharmacopoeia and British Pharmacopeia at 95%.
- 10 Kg fresh fruits of black currant (Ribes nigrum) are weighed on a technical balance and mixed with 10 L deionized water and 10 L ethylic alcohol 97 degrees of plant origin in the storage vessel.
- the mixture is homogenized with a mechanical homogenizer for 30 min., at room temperature, at a speed of 100 rpm.
- the suction pump hose is inserted in the storage vessel and the one for evacuation from reactor in the collecting vessel, the pump is coupled in order to supply with the continuous reactor and is turned on at a flow rate of 0.5 L/min.
- the ultrasounds sources are turned on at a power of 100 W/L and microwaves at a power of 300 W/L, the extraction time is set at 120 min.
- 3 Kg walnut kernel (Juglans regia L.) are weighed on a technical balance, milled at a graining of 0.6 mm and mixed with 6 L hexane in storage vessel.
- the mixture is homogenized with a mechanical homogenizer for 40 min., at room temperature, at a speed of 30 rpm.
- the suction pump hose is inserted in the storage vessel and the one for evacuation from reactor in the collecting vessel, the pump is coupled to supply with the continuous reactor, and is turned on at a flow rate of 0.2 L/min.
- the ultrasounds sources are turned on at a power of 300 W/L and microwaves at a power of 600 W/L, the extraction time is set to 60 min. After 60 minutes the mixture thus obtained is collected, which is separated by filtration from the plant material.
- the mixture of solvent and extracted fatty oil is distilled under vacuum in order to eliminate the solvent, rinsed 3 times with distilled water and dried on anhydrous
- the fatty oil thus obtained is stored in dark colour pots, at premises protected from light and heat.
- the extraction yield was calculated according to the Romanian Pharmacopoeia and British Pharmacopeia at 94%.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Acoustics & Sound (AREA)
- Physics & Mathematics (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
This invention refers to a process for extraction of active biological compounds from plants by simultaneous application of ultrasounds and microwaves in a laminar continuous flow regime of extraction, under conditions of a controlled flow regime, at temperatures which do not affect the structure of thermolabile active biological compounds and to a new type of chemical reactor for extraction of active biological compounds from plants, continuous, for carrying out this process. Also, the invention refers to an installation for continuous extraction of active biological compounds with the new type of chemical reactor for extraction. By the application of the process according to the invention there are obtained essential oils, fatty oils, blends of polyphenols, blends of anthocyanins, terpenes, sesquiterpenes compounds, stabilized proteins or in pure form which cannot be obtained by others techniques of extraction due to thermal degradation and/or structural degradation occurring during the process of extraction.
Description
Process and installation for extraction of biological active compounds from plants and continuous reactor for ultrasound and microwave assisted
extraction of biological active compounds from plants
Technical field
The present invention refers to a process for extraction of active biological compounds from plants by simultaneous application of ultrasounds and microwaves and a new type, continuous, chemical reactor for extraction of active biological compounds from plants provided with means for simultaneous application of ultrasounds and microwaves.
Also, invention refers to an installation for continuous extraction of active biological compounds from plants with the new type of chemical reactor for extraction.
Background art
There are known from literature many methods for extractions of essential oils from biological materials, through a variety of mechanisms and equipment configurations. Thus, the patent applications EP 1439218 A1, EP 1618798 A1, EP 1629725 B1, US 5002784 describe extraction processes of volatile oils from different types of plant materials and microwaves assisted devices for the related processes as described. Patent application EP 1439218 A1 describes an extraction process of natural volatile substances from biological materials by hydrodistillation by means of microwaves, without addition of solvent. Also, the patent application EP 1439218 A1 refers to a microwave extraction apparatus of volatile compounds from biological material by a hydrodistillation process, which comprises a microwave oven, with a microwave chamber for receiving the biological material and a condensation chamber wherein, the condensation chamber is situated above the microwave chamber and is connected to the microwave chamber through a channel bundle. This system improves the condensation and cooling area of the water vapours from outside of the microwave chamber. On the other hand, this extraction process takes place with relatively low yields and the extraction apparatus has a functioning in batch system, applicable for small quantities of biological material.
Another extraction method of the volatile oils from biological material consists of microwave application to biological material under low pressure conditions until the
natural substances are released from the biological material and followed by their condensation, as described in patent application EP 1618798 A1. Further, the application EP 1618798 A1 describes an apparatus with the following components: a microwave cavity with a receiving region of the microwaves, allowing a low pressure in microwave area and a condensation chamber, which are connected by a tube. Another extraction method of the volatile substances which have a low solubility in water, from biological material is described in the patent EP 1629725 B1. The extraction method as presented in patent, includes the following steps:
1) Introduction of biological material without solvent in the microwave cavity; 2) Irradiation of the biological material until it is released at least some of the natural substances of interest from the biological material;
3) Transportation of the natural substances by convection from microwave area to the cooling area;
4) Cooling of the natural substances until they are condensed;
5) Transportation of the released natural substances from the condensation area to the collecting area which contains a hydrophobic solvent for dissolution of natural substances.
The water carrying natural substances partially returns in the microwave area by a drainage system.
In secondary step the natural substances or the least soluble in water are separated from the hydrophobic solvent. The water vapours are generated inside the microwave cavity from the mixture water/biological material.
Another patent, US 5002784 describes a new method of selective extraction of natural compounds from raw biological material which requires a short time period for extraction and uses a microwave applicator. This method it is in concordance with all principles of conventional extraction, but in comparison with these ones the extraction yields are much better. The subsequent operations of separation and purification require special conditions.
All these extraction processes proceed at low speed and relative low extraction yields. It also does not allow obtaining polyphenols, anthocyanins and proteins and other thermolabile compounds.
Disclosure of invention
The technical problem solved by the present invention is given by the need to get a higher yield of extraction, with high purity of the extraction product, and to obtain also other valuable components such as polyphenols, anthocyanins, proteins, etc, whilst processing a much higher quantity of biological material.
The process of extraction of the active biological compounds from plants according to the invention solves this problem by simultaneous application of ultrasounds and microwaves to the plant material, in a continuous regime of extraction, in a controlled flow regime, at temperatures, at atmospheric pressure or vacuum and, if necessary, under inert gas atmosphere, which do not affect the structure of active biological compounds. Preferably, the controlled flow regime is a laminar regime (Re < 2300). Thus, a first object of the invention is a process for extraction of active biological compounds from plants which comprises the following steps:
- introducing the mixture of plant material and solvent, prepared in advance, in an extraction zone with controlled continuous laminar flow regime, the extraction zone being provided successively with means for the application of ultrasounds and means for the application of microwaves;
- applying simultaneously ultrasounds and microwaves to the mixture of plant material and solvent which goes through the extraction zone;
- volatile active biological compounds released in the extraction zone are collected in the condensing zone;
- cooling the volatile active biological compounds collected in the condensing zone until they condense completely;
- evacuating the mixture of plant material and solvent from extraction zone and separating the liquid extraction mixture containing solvent and non-volatile active biological compounds extracted from the exhausted plant material, which liquid extraction mixture is subjected to further processing appropriate for the separation of non-volatile active biological compounds from the extraction solvent.
In another embodiment of the invention, the mixture of plant material and solvent released from extraction zone is reintroduced in the extraction zone, recirculating so until all active biological compounds are extracted. Then, the liquid extraction mixture is separated from the plant material and is processed for obtaining the active biological compounds.
Another object of invention is a continuous reactor for extraction of active biological compounds, in the form of a pipeline, whose length is substantially higher than the diameter thereof and which assures a zone of extraction with a continuous flow regime, controlled, with supplying at one end and evacuation at the other end and which is provided with means for generating and simultaneous application of ultrasounds and microwaves and means for collecting the active biological compounds released in the extraction process.
Also, the reactor is provided with means for controlling and monitoring the temperature and working pressure, and the vacuum, the reflected and incident microwaves power as well as means for carrying out the extraction process under inert atmosphere, whenever this is necessary.
The reactor diameter is between 10mm and 2200 mm, depending of the operating manner, production capacity and the type of plant material which is subjected to the extraction process.
Another object of invention is an installation for extraction of active biological compounds from plants which comprises a continuous extraction reactor according to the present invention, connected to a circuit for the transportation of the mixture of plant material and solvent, which makes the connection from a storage vessel for the said mixture to the supplying end of the extraction reactor, and respectively, from the evacuation end of the extraction reactor, to the collecting vessel for the mixture and a pump for supplying the mixture in the extraction reactor.
The process according to the invention has many advantages: the quantity of biological material processed per charge is at least 100 times higher than in the batch system, the foaming phenomenon of the biological material is avoided and implicitly the undesired events, the extraction yield of natural substances increases by at least minimum 25%, the time of extraction is significantly reduced, it is obtained a product of high purity and high quality in terms of chemical composition compared to other methods and systems for extraction in a field of microwave and/or non- conventional methods, such as: extraction under pulsed electrical field, enzyme- assisted extraction, extraction with liquids under pressure, extraction with supercritical fluids.
The biological material subject to the extraction can be processed at the same time also for other valuable components, such as: polyphenols, anthocyanins, proteins, etc.
Also, the process according to the invention presents the advantages:
• Obtaining pure volatile oils;
• Obtaining of polyphenols, anthocyanins and proteins;
• Reduced time of extraction;
· Extraction temperature controlled depending on the extraction product desired to be obtained;
• Low temperature of extraction in order to avoid thermal degradation of thermolabile compounds;
• High volume of extraction;
· High yield of extraction ;
• Possibility of strengthening the electric or magnetic field of the microwave depending on the chemical nature of the «target» active biological compound;
• The extraction assisted by microwaves and ultrasounds is a fast, selective, non-polluting process, which works with a high speed of extraction, easy to control from a technological point of view.
Figure 1 represents schematically an embodiment of an installation of extraction of active biological compounds with the recirculation of the mixture of plant material and solvent to be extracted according to the invention comprising a continuous extraction reactor provided with means of generating and application of ultrasounds and microwaves and a system for collecting and condensing of active biological compounds resulted from the extraction process, connected to a transportation circuit for the plant material to be processed that makes the connection from a vessel for the said mixture to the supplying end of the extraction reactor, and respectively, from the evacuation end of the extraction reactor, back, to the vessel for the mixture and a process pump for supplying and recirculation.
Further it is presented the process according to the invention. It is selected the plant material to be processed for its content of active biological compounds.
The plant material may be in the form of plants, seeds, fruits, flowers, wooden material. The plant material is milled at a grain size which must not be greater than 20 pm or chopped if the plant material subjected to extraction is fresh.
The plant material may be fresh or dried.
In a storage vessel, it is prepared a mixture of plant material with solvent and it is homogenized so that the whole quantity of plant material, respectively plant, wood or seeds to be in contact with the solvent.
The mixing ratio, by weight, of plant material and solvent is dependent on the plant material to be extracted, shape, size, condition, and it is between 1 :2 and 1 :20, preferably between 1 : 2 and 1:10. The solvent may be polar or non-polar. Solvents used for extraction are chosen depending on the active biological compound pursued to be extracted.
For example, deionized water is suitable for extraction of essential oils, anthocyanins, tannins, saponins, terpenes, sesquiterpene.
Ethanol is a solvent suitable for extraction, for example, of alkaloids, terpenes, tannins, polyphenols, flavonoids.
Soybean oil, olive oil, coconut oil are suitable for extraction of fatty oils, terpene compounds, stabilized proteins. The mixture of plant material and solvent is supplied to a continuous extraction reactor by means of a process pump.
The reactor is provided with means for the application of ultrasounds, in the form of a sonotrod (US) and means for the application of microwaves, in the form of a multi- mode or mono-mode microwave cavity (MW).
Also, the reactor is provided with means for controlling and monitoring temperature and the working pressure, and vacuum, reflected and incident microwave power as well as means for ensuring carrying out the extraction process in an inert atmosphere, whenever this is necessary.
The reactor is connected to a drive system with steam of Clevenger type or Florentine flask for the collection and separation of volatile oil.
The ultrasounds and microwaves sources are turned on. The operational parameters are adjusted: time, temperature, vacuum level (where applicable), optionally, inert atmosphere, power of the ultrasounds, the incident power of microwaves, pump flow rate.
The work flow rate is correlated with the power of microwaves and ultrasounds applied to the mixture of plant material and solvent, namely: the greater flow rate it is the higher power of microwaves and ultrasounds are.
When the situation so requires, this proportion may be modified depending on the physical-chemical characteristics of the plant and/or the solvent and the rheqjogical characteristics of the mixture of plant material and solvent.
The mixture of plant material and solvent is subjected to simultaneous irradiation of ultrasounds and microwaves.
Power of ultrasounds sources is comprised between 100-1000 W/l and power of microwaves sources is comprised between 100-6000 W/l at a microwave frequency of 2450 MHz or GHz 914.
In an embodiment of the process, the mixture of plant material and solvent is simultaneously irradiated with ultrasounds and microwaves, ultrasonic power ranging between 100-500 W/l and microwave powers between 200- 000 W/l and a frequency of 2450 MHz, at an extraction temperature in the range of 40 to 110 °C, at normal pressure, the extraction time of 10-120 min and a flow rate of the pump of 0.1 to 2 l/min. The extraction of active biological compounds is accomplished under required technological conditions. Depending on the nature of active biological product obtained, namely: essential oil, blend of polyphenols, anthocyanins, or proteins, they are cooled at room temperature, they are conditioned by filtration, drying, centrifugation or lyophilization and they are stored.
By applying the extraction process according to the invention various active biological compounds are obtained comprising for example: essential oils, fatty oils, blends of polyphenols, mixtures of anthocyanins, terpenes, sequiterpenes compounds, stabilized proteins or in pure form.
There are further presented a few non-limiting examples for the application of the present invention.
Example 1
5 Kg dry Rosemary (Rosmarinus Officinalis) (EU origin) are weighed on a technical balance, milled at a graining of about 0.5 mm, introduced in the storage vessel, on which there are added 20 L deionized water, the mass ratio plant/solvent=1 :4.
The mixture is homogenized with a mechanical homogenizer for 30 min., at room temperature, at a speed of 50 rpm.
The pump suction hose is inserted in the storage vessel, the pump is cpupled in order to supply with the continuous reactor, and is turned on at a flow rate of 1 L/min. The ultrasounds sources are turned on at a power of 200 W/L and microwaves at a power of 400 W/L, the Clevenger system of collecting the volatile oil is coupled and the extraction time is set at 90 minutes. After 90 minutes the extraction of the vp!gtile oil has been completed. The volatile oil is separate^ from wafer apd jt is drj£d pn th
anhydrous Na2S04.The volatile oil thus obtained is stored in dark colour pots, at premises protected from light and heat.
In the collecting vessel of the plant material at the exit from reactor it is obtained an aqueous extract which contains antioxidant compounds. The aqueous extract is separated by filtration from the plant material and it is stored in dark colour pots for subsequent processing. A volatile oil and an aqueous extract are thus obtained. The gas chromatographic analysis of volatile essential oil of Rosemary has shown the main active compounds as presented in Figure 2.
The gas chromatographic analysis of aqueous extract of Rosemary has shown the main active compounds as presented in Figure 3.
The extraction yield was calculated according to the Romanian Pharmacopoeia and British Pharmacopeia at 95%.
Example 2
10 Kg fresh fruits of black currant (Ribes nigrum) are weighed on a technical balance and mixed with 10 L deionized water and 10 L ethylic alcohol 97 degrees of plant origin in the storage vessel. The mixture is homogenized with a mechanical homogenizer for 30 min., at room temperature, at a speed of 100 rpm. The suction pump hose is inserted in the storage vessel and the one for evacuation from reactor in the collecting vessel, the pump is coupled in order to supply with the continuous reactor and is turned on at a flow rate of 0.5 L/min. The ultrasounds sources are turned on at a power of 100 W/L and microwaves at a power of 300 W/L, the extraction time is set at 120 min. After 120 minutes the mixture containing the blend of extracted polyphenols is collected, which is separated by filtration from the plant material. The blend of polyphenols is concentrated by lyophilization. Thus obtained it is stored in dark colour pots at premises protected from light and heat. The extraction yield was calculated according to the Romanian Pharmacopoeia and British Pharmacopeia at 98%. Example 3.
3 Kg walnut kernel (Juglans regia L.) are weighed on a technical balance, milled at a graining of 0.6 mm and mixed with 6 L hexane in storage vessel. The mixture is homogenized with a mechanical homogenizer for 40 min., at room temperature, at a speed of 30 rpm. The suction pump hose is inserted in the storage vessel and the
one for evacuation from reactor in the collecting vessel, the pump is coupled to supply with the continuous reactor, and is turned on at a flow rate of 0.2 L/min. The ultrasounds sources are turned on at a power of 300 W/L and microwaves at a power of 600 W/L, the extraction time is set to 60 min. After 60 minutes the mixture thus obtained is collected, which is separated by filtration from the plant material. The mixture of solvent and extracted fatty oil is distilled under vacuum in order to eliminate the solvent, rinsed 3 times with distilled water and dried on anhydrous
The fatty oil thus obtained is stored in dark colour pots, at premises protected from light and heat.
The extraction yield was calculated according to the Romanian Pharmacopoeia and British Pharmacopeia at 94%.
Example 4
5 Kg shell of Palo Santo (Bursela Graveolens) are weighed on a technical balance and mixed with 10 L deionized water in a storage vessel. The mixture is homogenized with a mechanical homogenizer for 30 min., at room temperature, at a speed of 100 rpm. The suction pump hose is inserted in the storage vessel and the one for evacuation from reactor in the collecting vessel, the pump is coupled to supply with the continuous reactor, turned on at a rate of 0.3 L/min. The ultrasounds sources are turned on at a power of 250 W/L and microwaves at a power of 350 W/L, in a monomode system, the Florentine flask is coupled, the extraction time is set at 90 min. After 90 minutes, the volatile essential oil is collected in the Florentine flask, which then is separated from water by a separating funnel and dried on anhydrous Na2S04. Thus obtained this is stored in dark colour pots at premises protected from light and heat. There are obtained approximately 500 ml essential oil, with a yield of 98%. The composition of the oil is analysed by gas chromatographic-mass spectrometry method (GC-MS), the results being shown in figure 4. Example 5
5 Kg rose petals (Rosa X Damascena Miller) are weighed and mixed with 12 L deionized water in the storage vessel. The mixture is homogenized with a mechanical homogenizer for 30 min., at room temperature, at a speed of 100 rpm. The suction pump hose is inserted in the storage vessel and the one for evacuation
from reactor in the collecting vessel, the pump is coupled in order to supply with the continuous reactor, and it is turned on at a flow rate of 0.3 LJmin. The ultrasounds sources are turned on at a power of 150 W/L and microwaves at a power of 550 W/L, in a multimode system, the Florentine flask is coupled, the extraction time is set at 90 min. After 90 minutes the volatile essential oil is collected in the Florentine flask, which is then separated from water by a separating funnel, at 40-45°C and dried on anhydrous Na2S0 . The volatile essential oil thus obtained is stored in dark colour pots at premises protected from light and heat. There are obtained approximately 5 ml essential oil, with a yield of 95%. The composition of oil is analysed by GC-MS method and physical-chemical characteristics by specific standards, comparative results being presented in the following table:
Claims
1. Process for extraction of active biological compounds from plants characterized in that it comprises the following steps:
- introducing the mixture of plant material and solvent, prepared in advance, in an extraction zone with controlled continuous flow regime, the extraction zone being provided successively with means for the application of ultrasounds and with means for the application of microwaves;
- applying simultaneously ultrasounds and microwaves to the mixture of plant material and solvent which goes through the extraction zone;
- volatile active biological compounds released in the extraction zone are collected in the condensing zone;
- cooling the volatile active biological compounds collected in the condensing zone until they condense completely;
- evacuating the mixture of plant material and solvent from extraction zone and separating the liquid extraction mixture which contains solvent and non-volatile active biological compounds extracted from the exhausted plant material, which liquid extraction mixture is subjected to further processing appropriate for the separation of non-volatile active biological compounds from the extraction solvent.
2. Process according to claim 1 characterized in that the continuous flow regime is a laminar flow regime.
3. Process according to claim 1 characterized in that the application of
ultrasounds to the mixture of plant material and solvent which goes through the continuous extraction zone precedes the application of microwaves.
4. Process according to claim 1 characterized in that there are applied ultrasounds with the power comprised between 100 - 1000 W/l and microwaves with the power comprised between 100 - 6000 W/l and a microwave frequency of 2450 MHz or 914 GHz.
5. Process according to claim 1 characterized in that the powers of ultrasounds and microwaves applied to the mixture of plant material and solvent are determined as depending on the ratio plant material/solvent, the extraction temperature, the extraction time and the flow rate of the supplying pump.
6. Process according to claim 1 characterized in that the active biological compounds collected comprise essential oils, fatty oils, blends of polyphenols, blends of anthocyanins, terpenes, sesquiterpenes compounds, stabilized proteins or in pure form.
7. Reactor for extraction of active biological compounds, continuous, characterized in that it is in the form of a pipeline, whose length is substantially higher than the diameter thereof, which assures a zone of extraction with a laminar continuous flow regime, controlled, with supplying at one end and evacuation at the other end and which is provided with means for generating and simultaneous application of ultrasounds and microwaves and means for collecting the active biological compounds released in the extraction process.
8. The reactor according to claim 7 characterized in that the means for generating and application of ultrasounds are located before the means for generating and application of microwaves and in line with these ones.
9. Installation for continuous extraction of active biological compounds from plants characterized in that it comprises a reactor for extraction according to claim 7, connected to a circuit for the transportation of the mixture of plant material and solvent which makes the connection from a storage vessel for the said mixture to the supplying end of the extraction reactor, and respectively, from the evacuation end of the extraction reactor to a collecting vessel for the mixture and a pump for supplying the mixture in the extraction reactor.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP16740464.9A EP3283605A4 (en) | 2015-01-19 | 2016-01-18 | Process and installation for extraction of biological active compounds from plants and continuous reactor for ultrasound and microwave assisted extraction of biological active compounds from plants |
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| ROA201500035 | 2015-01-19 | ||
| ROA201500035A RO130896A0 (en) | 2015-01-19 | 2015-01-19 | Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants |
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| WO2016118034A2 true WO2016118034A2 (en) | 2016-07-28 |
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| EP (1) | EP3283605A4 (en) |
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| CN107930182A (en) * | 2017-12-29 | 2018-04-20 | 内蒙古金旭生物科技有限公司 | A kind of active substance of plant extraction element |
| WO2019068154A1 (en) * | 2017-10-02 | 2019-04-11 | Baldo S/A Comércio Indústria E Exportação | Process for producing roasted mate extract |
| CN111704961A (en) * | 2020-06-29 | 2020-09-25 | 山东省经济林管理站 | Walnut male flower essential oil and extraction method thereof |
| IT201900020630A1 (en) * | 2019-11-08 | 2021-05-08 | Univ Degli Studi Genova | Process and system for the extraction of molecules from solid particle matrices |
| KR20210086104A (en) * | 2019-12-31 | 2021-07-08 | 한국과학기술연구원 | Method of continuously producing cannabinol from Cannabis sp. and uses thereof |
| CN113563974A (en) * | 2021-08-19 | 2021-10-29 | 广州市藻德道科技有限公司 | Method for ultrasonically extracting ginger essential oil without organic solvent |
| WO2023187289A1 (en) | 2022-04-01 | 2023-10-05 | Innovation & Development Company | Microwave extraction oven for the continuous heat treatment of solid or pasty organic products |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1336968C (en) * | 1989-05-16 | 1995-09-12 | J. R. Jocelyn Pare | Microwave-assisted natural products extraction |
| FR2705035B1 (en) * | 1993-05-11 | 1995-08-04 | Archimex Pibs | Process and installation for solvent-free extraction of natural products by microwave. |
| RU2316375C2 (en) * | 2005-08-02 | 2008-02-10 | Общество с ограниченной ответственностью "Славянский чай" | Method for producing of dry water-soluble extract from raw plant material |
| CN102179062A (en) * | 2010-03-02 | 2011-09-14 | 上海远跃轻工机械有限公司 | Ultrasound/microwave continuous countercurrent extraction device and method |
-
2015
- 2015-01-19 RO ROA201500035A patent/RO130896A0/en unknown
-
2016
- 2016-01-18 WO PCT/RO2016/050001 patent/WO2016118034A2/en active Application Filing
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019068154A1 (en) * | 2017-10-02 | 2019-04-11 | Baldo S/A Comércio Indústria E Exportação | Process for producing roasted mate extract |
| CN107930182A (en) * | 2017-12-29 | 2018-04-20 | 内蒙古金旭生物科技有限公司 | A kind of active substance of plant extraction element |
| CN107930182B (en) * | 2017-12-29 | 2024-05-24 | 山西鑫旭生物科技有限公司 | Plant active substance extraction element |
| IT201900020630A1 (en) * | 2019-11-08 | 2021-05-08 | Univ Degli Studi Genova | Process and system for the extraction of molecules from solid particle matrices |
| WO2021090250A1 (en) * | 2019-11-08 | 2021-05-14 | Università Degli Studi Di Genova | Process and system for extracting molecules from solid particle matrices |
| KR102311749B1 (en) | 2019-12-31 | 2021-10-13 | 한국과학기술연구원 | Method of continuously producing cannabinol from Cannabis sp. and uses thereof |
| KR20210086104A (en) * | 2019-12-31 | 2021-07-08 | 한국과학기술연구원 | Method of continuously producing cannabinol from Cannabis sp. and uses thereof |
| CN111704961B (en) * | 2020-06-29 | 2022-04-08 | 山东省林业保护和发展服务中心 | Walnut male flower essential oil and extraction method thereof |
| CN111704961A (en) * | 2020-06-29 | 2020-09-25 | 山东省经济林管理站 | Walnut male flower essential oil and extraction method thereof |
| CN113563974A (en) * | 2021-08-19 | 2021-10-29 | 广州市藻德道科技有限公司 | Method for ultrasonically extracting ginger essential oil without organic solvent |
| WO2023187289A1 (en) | 2022-04-01 | 2023-10-05 | Innovation & Development Company | Microwave extraction oven for the continuous heat treatment of solid or pasty organic products |
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Also Published As
| Publication number | Publication date |
|---|---|
| RO130896A0 (en) | 2016-02-26 |
| EP3283605A4 (en) | 2018-11-14 |
| EP3283605A2 (en) | 2018-02-21 |
| WO2016118034A3 (en) | 2016-10-06 |
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