OBTAINING A JUICE OF FRESH PLANTS BY THERMOMECHANICAL TREATMENT AND COSMETIC AND THERAPEUTIC USE THEREOF

The present invention relates to a method for obtaining a fresh plant juice, wherein said fresh plants, excluding seeds alone, are subjected to thermomechanical treatment in the absence of solvent, followed by a recovery operation of the juice.

Means widely described a juice fresh plant produce consists of a pressing process or further comminution and centrifugation.

Patent ep0279984 describes the cosmetic use of a juice of plants of the family Gramineae obtained after an extraction by crushing, grinding and/or crushing of the plant.

Except fruits, juices of medicinal plants are also implemented.

Some techniques are aimed potentiate the extraction of components of the membrane, such as "a flash trigger", technique widely used for grapes, for increasing the extraction of anthocyanins.

The method said integral suspension system fresh plant produce (SIPF) provides fresh plant juice in particular by a step of cryomilling to -25 °c then -196 °c and maceration of the powder obtained in an alcoholic solution.

Processing said thermomechanical treatment is by mechanical energy under conditions of particular temperatures and adapted. Examples of mechanical energy are among others: pressure, milling, extruding, andc.

The extrusion is a process whereby a material flowable under various controlled conditions is then constrained to pass in a die at a determined speed (Dziezak, J.D. (1989). Twin screwextruders its single NDA concentré both in technical jargon. Concentré SCI, april-, 164 - 174). Initially, this technology has been used in the metallurgical industry, in England, at the end of the century 18ième. Some time later, it was placed in the agri-food industry for making sausage, and pasta. Today, the food industry uses abundantly extrusion technique through the extrusion cooking of the starch products (cookies, rusks, snack foods, and so on) but also the texturing proteins and the production of foodstuffs for farm animals or pets.

Parallel, extrusion technology has been widely developed for the thermoplastics industry, and has lead to the design of new screw, a development of the technology and opening to new applications.

A number of studies have thus carried on the use of the extruder to perform actions chemical, mechanical, thermomechanical in a single step and continuously, such as the extraction of hemicelluloses (not Diaye, sec., Rigal, L., technical specifications, e., Clarke, f.w., 1996. Extracting hemicellulose from-OC Planting Poplar TENs, for practical year-type twin screw extruding protective measures: A fFeasibility Study. Bioresearch Hub 57, 61 - 67) (only Diaye sec., given our limited experience in the alkaline Rigal L OC extracting hemicellulose Planting tea in a biological twin screw protective measures: correlating avec la arrest specific resident of Mechanical canadien Time Division dispensing of imprinted blocking liquid-phase (2000) Bioresource Hub, 75 (1), ρρ. 13 - 18), pectins (Marshal V, Rigal L of covalent bypass relationship has OC - sunflower crop stalks zu business application (1999) NDA densiflorum Advanced Industrial Forage NDA Agri, 10 (3), ρρ. 185 - 200). and so on. in such cases, an acidic or basic solvent is introduced into the extruder at the same time as the plant raw material, to facilitate extraction and solubilization macromolecules searched (reactive extrusion).

Some applications are already known in the extraction plants: the implementation of the single screw extruder for expression of oils from oil seed with which solvent is not injected into the sheath, this oil extraction based only on compression of the solid (Sriti J, Talou Τ ., Faye board m, Vilarem g Marzouk B diesel oil extracting DNA from-coriander fruit bypass extruding NDA resettable with a comparison based solvent extracting the processes. (2011) Advanced Industrial Forage NDA Agri, 33, 659 - 664).

The extrusion is also used as a pretreatment, on marc of fruits (apple, blackcurrant, cranberry..) in association with a solid support such as corn starch, in order to increase the extraction of phenolic compounds (1995 Brittany Bonish L, Cascade excited L, at Prior Dr. Ronald L Polyphenolicantioxidant NDA. the composition extruded of Fisheries pomaceous cranberries. (2010), J agriculture. Appl. 58, 4037 - 4042.) (RC-Khanal, Cascade Ir, at Prior LAN. Procyanidin of Trace Based on seed-NDA pomaceous, improvement plans and anthocyanin of Trace Based pomaceous aces significantly poorer extruding technical jargon. (2009) J. concentré IBS, 74: Η 174 - 82).

Some patents mention the juicing fresh plant produce by extrusion, extrusion hear an auger for conveying the plant with a piston compressor. The illustrations show a single shell with a single screw (su1669978, su1541071, su1518142, su496193, su3986103).

Another Patent made mention of a method for producing a juice from fresh plants, with as pretreatment before pressing or filtration or grinding the plant under inert atmosphere, either bursting by vacuum extrusion. However the extrusion is not here the means for extracting the juice, but preparing the plant before extraction (ep906113).

The request wo2012/098167 describes the juice to be obtained cannabis and its use as a beverage, listing as an example of a cold extrusion process. The aim here is to preserve the most nutritional qualities of the plant:

amino acids, proteins, vitamins. The pressure of the fresh for obtaining the juice is carried out at temperatures between 10 and 40 °c. It is therefore not mentions here thermo-mechanical processing.

The state of the technique may be further supplemented by the citation of the documents:

• U.S. 5,403 613 (D1)

• W097/33596 (D2)

. Wo2012/098167 (d3), and

· GalatheaBisterfels to von DREE, "Juice from-cannabis material seedlings zu concentré/wave, assists in gold biogaz" (d4).

U.S. 5,403 613 describes a process for making carrot juice by extraction with an aqueous solution of citric acid or lemon juice involving a heating step. The juice is then recovered by passing through a counter-rotating twin-screw extruder.

W097/33596 and wo2012/098167 describe other methods of extracting juice from various plants, to obtain the extract in powder form involving the addition of mono - or di-saccharides and for obtaining a cannabis-based, respectively.

Finally, "Juice from-cannabis material seedlings zu concentré/wave, assists in gold biogaz", described extracting juice from cannabis without however can be interested if necessary to the thermomechanical treatment in the absence of solvent to inactivate endogenous enzymes while preserving the molecules of compounds of interest without any native form.

It is important to recall that during the pressing of fresh plant, the plant wall brakes sometimes the recovery of certain compounds of interest, hence can be extracted either by means of an organic solvent, either after enzyme treatment. In addition, the enzymes are easily released and can begin to change the compounds extracted in the juice: hydrolyzed, oxidations, déglycosylations, andc..

Surprisingly and unexpectedly, adapting a extrusion technique widely used in food for cooking and expanding materials, for extraction purposes has recovered by a natural extract of the fresh. This fresh plant juice obtained by the present invention can directly be used in cosmetic or therapeutic.

By "extruder" is meant according to the present invention a thermomechanical treatment comprising extruding the fresh in an extruder, preferably a twin-screw extruder, associated with a heat treatment.

In one embodiment, the extrusion is characterized by the passage of the fresh in a twin-screw extruder compound:

an insertion region - fresh plants: feed hopper

- the main body of the extruder is comprised of one or more sheaths in which rotate the augers (-rotating or counter-rotating), or screw segments. Preferably, this will more successive adjacent sleeves. Of

preferably, these two five-year worm-rotating. The profile of the screws may vary with the shape of the thread of the screw (e.g. trapezoidal, conjugate, single or double...) and of the pitch. Each of the pedicle screws may also have different sections (or segments) which may possibly differing from one another, by the thread form and/or by the flighting. Optionally, one portions constituting the screw can also correspond to elements monolobes churns, trilobal or;

at least one sheath - filter:

S occurs if necessary for separating solid/liquid;

the V ' further comprises a filtering means, such as a grid, and;

the V ' is in particular located at the outlet of the extruder;

- means for heating and cooling because the sheath must be temperature-controlled: 60 to 300 °c of.

means for piloting the extruder such as:

the V ' a group drive: compound gear motor and a torque divider, which provide the mechanical power required to spin the screws;

the V ' automata piloting: allow monitoring and control of the process. The parameters that can be adjusted are: the speed of rotation of the screws and the temperature of each pod.

In a particular embodiment, the extruder is a twin-screw extruder to rotating screws and copénétrantes.

In another particular embodiment of the invention, the method involves an extruder and preferably a twin-screw extruder, to more sheaths and terminated by a sheath filter, for varying the temperature and at the same time apply shear, intense mixing of the plant raw material, with the consequence of causing a large number of compounds, break down the material but also inhibits the endogenous enzymes simultaneously by a thermal treatment.

The method according to the invention involves extruding plants fresh or frozen to extract juice, followed by a recovery and purification (collection) of the juice and finally into a final optional step, stabilize the juice collected.

The present invention therefore provides a method of obtaining a fresh plant juice, excluding the grains only, thermomechanically processed fresh plants are extruded in an extruder, associated with a heat treatment for inactivating the endogenous enzymes and keep the molecules of compounds of interest in the native form, in the absence of solvent, followed by a recovery operation of the juice.

According to a feature of the invention, the juice recovered is subjected to a later stage of stabilization, clarification and/or filtration.

According to another feature of the invention, the thermomechanical treatment has the steps trituration by shear at temperatures between 60 °c and 300 °c, preferably between 60 °c and 120 °c.

Advantageously, the thermomechanical treatment is carried out in a twin-screw extruder having a first area two-rotating screws and copénétrantes which effects the trituration of said plants and a second area separated twin-screw which effects the solid/liquid separation. The flow in the area twin-screw is generated by a pumping effect and not by friction forces arise between screw and sheath as viewed in a single screw extruder.

According to another feature of the invention, said first area is twin-screw located on the supply side of the extruder in fresh plants and said second area twin-screw is located on the side of the outlet of the extruder.

Advantageously, each of said zones comprise at least one sleeve and preferably several successive adjacent sleeves.

An additional feature of the invention, the different sleeves have control means and temperature control and means for heating and/or cooling.

According to a preferred characteristic of the invention, the twin-screw extruder comprises at least one filter sleeve.

According to another feature of the invention, the heating means are constituted by a heating collar preferably disposed in the first area.

Advantageously, the power supply, the transportation, the mechanical shearing and the thermomechanical treatment for crushing plants and fresh juice extraction are performed in the first zone of the extruder, and the solid/liquid separation operation is performed in the second area.

Advantageously, the first area comprises several successive sleeves whose temperatures are adjusted to have stages temperature rising staggered between 60 °c and 120 °c, and the second region comprises at least one sleeve carried at a temperature of between 30 °c and 120 °c, preferably between 30 °c and 100 °c.

By "fresh plant" is meant according to the present invention all or part of plant, excluding the grains only, used fresh or frozen (die), 30 to 80% composed of water, preferably 30 - 90%.

By "plant part", is meant in particular the aerial parts such as rods, bows, leaves, fruits and/or flowers; and/or the subterranean parts such as rhizomes, roots and/or bulbs.

In one particular implementation of the invention, whole plants being used.

Among the plants which can be used in the present invention, include among others: Of Avena sativa, Lonicera officinalis extract, fromTropaeolum majus, Echinaceaesp., Urticadioica, Plantago majorsp., Retroflexus Taxus canadensis, arvense, ofCalendula officinalis, Melissa officianalis, angulatasp., Cellulis vaccinium, Sambucus with lots, with Zingiber officinale and/or Turmericsp., Betula-sp., Of Menthasp., Althaeasp., the poaceae, Asteraceae and/or Labieae and preferably Of Avena sativa, Echinaceaepurpurea, Urticadioica, Plantabo lanceolata Buckhorn, arvense.

In one particular implementation, this will of: Of Avena sativa (Oats, aerial parts), Lonicera officinalis L. (Sweet clover, aerial parts), FromTropaeolum majus (Nasturtiums, flowering aerial parts), Echinaceae in SP. (Echinacea, flower heads), Urticadioica (nettle, aerial parts), Plantago major in SP. (plantain fruits, aerial parts), Taxus canadensis retroflexus (fleabanes Canada, aerial parts), Arvense (horsetail, aerial parts), OfCalendula officinalis (OfCalendula, flowers), Melissa officianalis (Balm, aerial parts), Angulata in SP. (fruit), Cellulis vaccinium (fruit), Sambucus with lots (fruits and/or flowers), With Zingiber officinale (Ginger, the rhizomes) Betula- in SP. (Birch, sheets) and/or Turmeric in SP. (rhizome).

In one preferred implementation, fresh plants are selected from the following group corresponding to plants having the active constituents are more sensitive to degradation by endogenous enzymes, such as polyphenoloxidases, peroxidases, myrosinases, 3-glucosidase, lipoxygenase:

Of Avena sativa

FromTropaeolum majus

Echinaceae SPs.

- Urticadioica

Plantago major in SP.

Urticadioica

Of Mentha in SP.

Melissa officianalis

- Betula- in SP.

Poacea

Aesteraceae

Labieae.

In another particular embodiment of the invention, matched plantlets of oats.

By "plantlets oat", is meant in the sense of the present invention oats before heading, c'est to say stage after germination (about 2 weeks to 2 months after germination) during the stage of the run-up to the heading not included. So-called "run-up" the growth phase which corresponds to the elongation of the rod and to the rising of the corn to forming, before flowering. Secondary metabolites are included herein wo2010/054879 as components of an extract of plantlet oat: flavonoids and saponins avenacoside-type.

In one embodiment of the invention, the harvested goods are stored intermediately to 4 °c for transportation to a freezing tunnel to

-40 °C.

The moisture content of the plants must be at minimum of 30% for a full performance of the technique.

This allows for work on fresh plants which has not been drying step, maintaining fact their native molecules. The extraction is carried out without a solvent, the process is very rapid, the residence time of the plant in the extruder can range from a few seconds to minutes and preferably between 10 seconds and 5 min, continuously, and flow rates of treatment varies depending on the size of the extruder of 20 to 500 kg/H of plant, corresponding to the obtaining of 10/hr to 300i juice.

The mechanical method of bicomponent extrusion screw causes the formation of a plug plant giving a pressure to the material and a bursting of cells, a destructuring of the plant material for recovering a high content of active compounds, even poorly water soluble. This provides an important advantage with respect to a pressing single or to a single screw extruder.

In addition, temperature changes during the extrusion step for fluidizing the mixture grounds juice of plant and thus improve performance in cases where the juice is thick due to the presence of mucilage. The temperature of the applied method can also inactivate endogenous enzymes and keep the molecules in their native form. This is very important for certain compounds which are rapidly inactivated as e.g. glucosinolates degraded by myrosinases (Cruciferae), caffeic acid derivatives oxidized by polyphenol oxidases (echinacea) (Nüsslein B, Kurzmann m, Bauer on R, Kreis Administration W Enzymatic degrading d'Cichoric acid is also in-dry Echinacea purpurea formulations (2000) J nats. Drug production ., 63, ρρ. 1615 - 1618), activated by a certain phytoalexins déglucosidases (Avenacosides in oats)... (Morant's NV, Jørgensen Κ ., Jørgensen C, M.S. unilaterally, Sánchez-to-Pérez R, Moller HJ Shipments, Backup sec. 3-glucosidase aces detonators d' seedling of Chemical defending (2008) Phytochemistry, 69 (9), ρρ. 1795 - 1813).

Collecting the juice of splitting the juice of interest solid residues can then take place by clarifying and/or filtration.

By "clarifying" is meant removing cell fragments present in the juice to the outlet of the extruder. This removal can be done by the technical clarification by centrifugal effect, which aims at eliminating the solid residue which could clog the filter medium. This removal can also take place directly by filtration with an adjuvant.

By "filtering" is meant end filtration or tangential, where it is contemplated the presence of filter aid (perlite, diatomaceous earth, and so on.). This filtration can retain the last residue solids, with the purpose of achieving a solution perfectly clear. It can be followed by filtration on membrane with a cutoff threshold set according to the size of the molecules to be considered. It can also be replaced or followed by filtration on silica or resin, to enrich for the compound of interest (e.g.: adsorption resins).

In a particular embodiment, the clarification step - filtering will be performed using a sleeve filter integrated end-extruder.

By "stabilization", is meant according to the present invention:

- for the supply of a liquid extract:

S cooling and then freezing juice

S treatment of juice by sterilizing filtration on 0.22 MW, pasteurization, sterilization uu.h.t, ultrafiltration and preservation in a package adapted avoid being contaminated posterior treatment: pockets vacuum filled sterile, single-use sterile containers.

O the storage can take place at room temperature, 4 °c to -20 °c (freezing) or.

O it will also consider the addition of preservatives (such as glycols, or sorbic acid, citric, andc) or alcohol (15° to a minimum).

- for providing an extract from pasty: concentrations in order to obtain a dry matter content greater than or equal to 65%.

- for the supply of a dry extract, technologies of vacuum drying, lyophilization or atomization may be envisioned.

The extracts obtained, liquid, pasty or dry as defined above can be used as it is in conventional cosmetic, pharmaceutical or food, intended to be administered topically or orally.

The main advantages of the method according to the invention over existing methods (pressing and single screw extruder) consist of:

- yield of juice in relation to the fresh material engaged (juice/weight of the fresh material engaged); and/or

- obtaining the juice richer in compounds; and/or

- obtaining the juice containing molecules not degraded by enzymes released during the crumpling of the fresh.

Example 1

12.75 kg of fresh aerial parts (12:00 PM to 2 °c) thawed oat (. Of Avena sativa L.) the forage harvester harvested after 2 months of growth (oat seedlings) have been introduced in the first sheath of a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} Bc45 which has 5. The temperature applied to the different sheaths is of 30 °c/120 °c/120 °c/120 °c/60 °c.

The scheme of the method is established as follows (total duration of the extrusion step=20 minutes; throughput 38 kg of plants/H and 22 kg/hr juice):

Fresh aerial parts==120 °c extruding>>extruded grounds

=>raw juice (57.2% yield (p/p))

=>clarifying

=>sterilizing filtration

41

Clear juice containing 11% dry matter (msec)

(53.1% yield (p/p))

=>5.8% fresh plant/msec

After extrusion, 57.2% p/p juice is obtained with respect to the material engaged. Clarification steps and sterilizing filtration were then performed to obtain a clear juice, with a final yield of 53.1% juice containing 11% of dry matter, or a yield of removed solids of 5.8% (p/p).

The yield of juice obtained by pressing (grinding - pressing - filtering) the same basic material is 50%, containing 4.5% of dry matter, is 2.25% yield (p/p).

Extrusion technology makes it possible to provide more juice, juice and a richer in compounds, and in particular a bioactive compound. Indeed, the flavonoid content of the juice obtained according to example 1 is 0.26%, while it is only 0.02% in the juice obtained by pressing with the same raw material. The flavonoid content therefore has been multiplied by 10 in this case.

We can also recognize the interest of melt extruding the flavonoid content for: the temperature remove more than compounds (of which four times more flavonoids) and obtain the native molecules, non-denatured by the enzymes.

This is also that he or she is with the saponins of oats, the avénacosides, which are rapidly déglucosylées by pressing. The native molecules are retrieved only by thermomechanical treatment: juices obtained by extrusion 120 °c to 200 °c and contain much avenacosides (a and b) to height of 89 mg and 100g for 93 mg of dry matter. They have heretofore not been degraded by endogenous desglucosidases.

Example 2 :

3.14 kg of heads of echinacea (dry Echinacea purpurea (L) reminisced) fresh thawed (6:00 PM to 2 °c) are fed into the first barrel of a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} Bc45 which has 5. The temperature applied to the different sheaths is of 100^{the O} C/100 °C/100/100 °C^{the O} C/60 °C. The process and material balance are shown in the table below (total duration of the extrusion step: 25min; throughput 7 kg of plants/H and 3 kg/hr juice);

After extrusion, we have therefore obtained 48.1% p/p juice than the material engaged. Clarification steps and filtration were then performed to obtain a clear juice, with a final yield of juice containing 10.09% 25% dry matter, either a dry content of 2.5% yield (p/p).

The caffeic acid content of the juice is:

cichoric acid: / 1.7% dry matter, is 0.17% p/v

caftaric acid: 1.21%, 0.12% p/v either

When the juice is extruded at room temperature, the content of citric acid and caftaric is almost zero due to action of the enzymes. When the juice is obtained by pressing of the head fresh, the content of these molecules is also zero.

Indeed, the enzymes released during the pressing (phenol oxidases) will rapidly oxidize these molecules (Nüsslein Β ., Kurzmann m, Bauer on R, Kreis Administration W Enzymatic degrading d'Cichoric acid is also in-dry Echinacea purpurea formulations (2000) J nats. Drug production ., 63, ρρ. 1615 - 1618, R Bauer on Medicare d' dry Echinacea purpurea tags Juice to all who Cichoric acid is also NDA Alkamides, Journal of Herbs, cellar & Medicinal Plant v. 6, the ISS. 3, 1999).

When the extrusion is performed at room temperature or at 60 °c < , the enzymes are not inactivated and will degrade the molecules of interest. In this example, only the extrusions made 100 °c or 200 °c can extract the plant, without degradation, and caftariquescichoriques acids (see summary table).

Most of the echinacea juice on the market do not contain these molecules, only the extracts obtained in the alcohol of aerial parts dry have active compounds

We also note that the extrusion process, never used as the only solvent that water naturally present in the plant, makes it possible to extract much more compounds of interest that an aqueous extraction.

REPLACEMENT SHEET (RULE 26)

Example 3 :

5.11 kg of fresh aerial parts (8:00 PM to 2 °c) thawed balm (Melissa officianalis L) are fed into the first barrel of a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} Bc45 which has 5. The temperature applied to the different sheaths is of 120 °c/120 °c/120 °c/120 °c/60 °c. The process and material balance are shown in the table below (duration of the extrusion step: 7 minutes; throughput 46 kg of plants/H and 29 kg/hr juice);

Under these conditions, extruding a juice with near 50% of yield and containing 6.5% of dry matter. This material contains between other rosmarinic acid, usually extracted by hydro-alcoholic mixtures such as ethanol 70%. The rosmarinic acid content in the removed solids by extrusion, without organic solvent, is here of 2.4% (p/p), which is comparable to a 70% ethanol extraction.

Example 4 :

4.5 kg of fresh ginger rhizome (Zingiber officinale and Canoe) are fed into the first barrel of a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} BC45. The temperature applied to the different sheaths is of 60 °c/60 °c/60 °c/60 °c/60 °c. The process and material balance are shown in the table below:

(total residence time in the extrusion step: 5 minutes; throughput 54 kg of plants/H and 32 kg/hr juice)

Example 5 :

5.32 kg fresh rhizomes of Curcuma (From Curcuma longa L) are introduced into le first sheath with a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} BC45. The temperature applied to the different sheaths is of 120 °c/120 °c/120 °c/120 °c/120 °c. the process and material balance are shown in the table below (total duration of the extrusion step: 10 minutes; throughput 32 kg of plants/H and 13 kg/hr juice).

The juice obtained is not filtered to retain the lipophilic compounds extracted by extrusion, suspended: curcumin and derivatives.

The assay shows that their content in the juice obtained is large (8.36%), greater than a juice solids present in the juice commercially sold (4.52%, containing juice turmeric, citric acid).

: CID=instantaneous controlled pressure

20.5 kg of fresh aerial parts of thawed Of Plantago lanceolate (76% moisture) are fed into the first barrel of a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} Bc45 which has 5. The temperature applied to the different sheaths is of 120 °c. 43.8% juice are obtained as it leaves the extruder. The process and material balance are shown in the table below:

A step d'ultra-filtering gave a juice better organoleptic quality. This juice contains 6.2% of dry matter. These solids contains assets of interest, iridoids (1.8%) and phenolic acids (0.3%). These values are very close to those obtained with an aqueous-alcoholic extract EtOH30 %, and greater than an aqueous extract. This gives free extract solvent quality equivalent to an aqueous-alcoholic extract.

18.8 kg of aerial parts fresh thawed than1 ' Urticadioica (76% moisture) are fed into the first barrel of a twin-screw extruder to rotating screws and copénétrantesCLEXTRAL^{the MC} Bc45 which has 5. The temperature applied to the different sheaths is of 120 °c. 9.4 kg of juice are obtained as it leaves the extruder, corresponding to 50% of yield.

This juice, containing 5.7% of dry matter after centrifugation, can be used as is, after pasteurization.

Example 8 : capsule

Melissa leaf juice in example 3, 200 mg lyophilized

45 Mg starch

Magnesium stearate 2 mg