FR3156664A1 - Process for manufacturing a composition - Google Patents

Abstract

To make a composition, malt roots are provided, and an extract is obtained by microwave-assisted extraction of the malt roots dispersed in a solvent.

Description

Process for manufacturing a composition FIELD OF THE INVENTION

The present invention relates to methods of manufacturing compositions.

More specifically, the invention relates to a method of manufacturing a composition from barley rootlets.

TECHNOLOGICAL BACKGROUND

During the malting process, the conditions necessary for the initiation of cereal germination are reproduced. A rootlet then grows from the grain. During a subsequent degerming stage, the grain is separated from the rootlet. The grain is then recycled. The rootlet remains a significant by-product (around 3 to 5% by mass) of the malting process, which we seek to recycle.

Until today, in industrial processes, the rootlets from the malting process are used as corks.

However, we are seeking to identify new ways to effectively use these rootlets.

Thus, the invention relates to a method of manufacturing a composition comprising:
- we provide malt rootlets,
- an extract is obtained by microwave-assisted extraction of malt rootlets dispersed in a solvent.

This extraction makes it possible to obtain an extract comprising a source of compounds sought in certain applications, such as, for example, nutrition, aromatics or cosmetics.

The extraction implemented makes it possible to preserve molecules of interest present in the rootlets, and even to produce them in sufficient quantities so that it is possible to implement the extraction process on an industrial scale, in order to provide these compounds in an efficient, reliable, reproducible and economically viable manner.

Depending on different aspects, it is possible to predict one and/or the other of the characteristics below taken alone or in combination.

According to one embodiment, the malt is a malt of barley, wheat, rye, spelt, corn, millet, sorghum, oats, triticale or rice, in particular a barley malt.

According to one embodiment, the composition obtained comprises polyphenols.

According to one embodiment, the composition obtained comprises flavonoids.

According to one embodiment, the composition obtained comprises flavonols, flavanols, isoflavones, flavones, flavanones and/or anthocyanins; or polymers thereof, in particular proanthocyanidols.

According to one embodiment, the composition obtained comprises non-flavonoids.

According to one embodiment, the composition obtained comprises curcuminoids, lignans, phenolic acids and/or stilbenes.

According to one embodiment, the composition obtained comprises quercetins, kaempferols and/or catechins; and/or condensed tannins, such as procyanidins and/or prodelphinidins.

According to one embodiment, the composition obtained comprises hydroxybenzoic and/or hydroxycinnamic amino acids, in particular ferulic acid, caffeic acid, sinapic acid, o-coumaric acid and/or p-coumaric acid.

According to one embodiment, the composition obtained comprises phenolamides, such as for example hordatines, in particular hordatine A, hordatine B, and more particularly hordatine B1, hordatine C and/or hordatine hexoside, and more particularly hexoside B and/or hexoside B1.

According to one embodiment, the composition obtained comprises coumaroyl hydroxyagmatine.

According to one embodiment, the composition obtained comprises feruloyl hydroxyagmatine.

According to one embodiment, the composition obtained comprises phenylethylamine, in particular alkaloid, in particular hordenine.

According to one embodiment, the solvent is water, alcohol, or is hydroalcoholic.

According to one embodiment, the solvent is acidic and has a pH preferably between 1 and 5, in particular between 2 and 4, more particularly between 2.5 and 3.5.

The inventors found that, surprisingly, extraction in an acidic medium caused a significant increase in the extraction yield and, even more surprisingly, while preserving the compounds of interest present in the malted barley rootlets. Thanks to these provisions, it therefore becomes possible to obtain one or more compounds of interest from the malted barley rootlets in an economically feasible manner.

According to one embodiment, the microwaves are emitted at a frequency of 915 MHz at a power of between 1 and 100 kW.

According to one embodiment, the microwaves are emitted at a frequency of 2,450 MHz at a power of between 1 and 25 kW.

According to one embodiment, before implementing the extraction, a selection of a fraction of the rootlets is carried out according to their dimensions and/or their density.

According to one embodiment, a hydro-alcoholic extraction is also implemented after the microwave-assisted extraction.

According to one embodiment, sterilization, in particular gentle sterilization, is carried out before microwave-assisted extraction.

According to one embodiment, post-processing of the extract obtained is also carried out.

According to one embodiment, the malt rootlets are supplied in the form of ground material and/or a fraction of ground material.

According to one embodiment, before supplying the rootlet, the raw material is cleaned, said cleaning involving at least one sieving and/or one densitometric separation.

DETAILED DESCRIPTION

Definitions

"Malt" here refers to a sprouted cereal obtained by a malting process. Malt can be obtained by any suitable malting technique. Malting typically takes place in 4 stages, including steeping, which moistens the grain; germination, during which the grain begins to sprout and gives rise to "green malt," roasting, during which the green malt is dried to obtain dry malt, and degerming, which separates the malt from its rootlets.

The term "rootlets" refers to so-called "sieved" malt rootlets that are at least free of acrospires, grain husks, dust or fragments thereof, and their mixtures present in the coarse product generated during the malting process. The malt rootlets may have been obtained after 3 to 11 days of germination. The malt rootlets may be obtained from a cereal malt, and in particular from malt selected from barley, wheat, rye, spelt, corn, millet, sorghum, oats, triticale, rice and their mixtures. The malt rootlets are typically prepared from barley malt and/or wheat malt.

Barley (hordeum vulgare) is a straw cereal, an annual herbaceous plant of the Poaceae family, Pooideae subfamily.

The rootlets resulting from the separation process typically have an elongated shape. The characteristic size thereof is its length. In the context of the present invention, the sieved rootlets have a length of less than 2.5 millimeters (mm), in particular less than 2 mm, in particular less than 1.5 mm, in particular less than 1 mm, in particular less than 0.75 mm, in particular less than 0.5 mm, in particular less than 0.25 mm. In the context of the present invention, the sieved rootlets have a length of greater than 0.125 mm, in particular greater than 0.25 mm, in particular greater than 0.5 mm, in particular greater than 0.75 mm, in particular greater than 1 mm, in particular greater than 1.5 mm, in particular greater than 2 mm.

The term “ground material” refers to a powder-like material obtained by grinding and/or sieving a solid agricultural product. In the context of the present invention, the “ground material” is characterized, among other things, by its particle size and its density. In the context of the present invention, the ground material has a particle size of less than 0.5 mm, in particular less than 0.25 mm. In the context of the present invention, the ground material has a particle size greater than 0.125 mm, in particular greater than 0.25 mm, in particular greater than 0.315 mm. In the context of the present invention, the ground material has a density of between 0.2 and 0.5, for example between 0.2 and 0.35, between 0.35 and 0.5, or between 0.3 and 0.4.

The table below shows the dispersion of grain sizes of malt rootlets (sieved raw material) and ground material thereof typically used in the context of an embodiment of the invention. Fraction Sieved raw material Crushed sieved raw material >500 micrometers (µm) 0.71 0.50 >315 µm 43.60 38.60 >250 µm 23.46 30.40 >125 µm 27.25 26.70 >80 µm 1.85 1.90 Bottom 3.44 1.90

[Table 1]: Particle sizes (mass percentage)

“Hydrolysis” refers to a chemical and/or enzymatic reaction in which a covalent bond is broken by a water molecule.

The term "Polyphenol" refers to an organic molecule comprising at least one, and in particular at least two, phenolic groups, and generally of high molecular weight. These natural molecules, very widely present in the plant kingdom, are therefore also found in human and/or animal food. In the context of the present invention, polyphenols are considered to have an antioxidant function.

Flavonoids are a class of polyphenolic compounds with a basic structure consisting of two aromatic rings linked by three C6-C3-C6 carbons. Flavonols, flavanols, isoflavones, flavones, flavanols, and anthocyanins are part of the flavonoid class. In particular, flavanols can be considered to have an antioxidant function. In particular, flavonols include quercetin or quercetol, kaempferol, and/or catechin, and can be considered to provide an antioxidant function.

Coumarin refers to the class of phenolic compounds derived from 2H-1-benzopyran-2-one.

The term "non-flavonoids" refers to a class of polyphenolic compounds including, among others, curcuminoids, lignans, phenolic acids and their derivatives, stilbenes and tannins.

Among the tannins are proanthocyanidols.

Among the proanthocyanidols, "procyanidin" refers to a family of condensed tannins formed by flavanol units of the catechin and epicatechin type.

Among the proanthocyanidols, “prodelphinidin” is a condensed tannin of catechin.

Malt, and in particular barley malt, may comprise procyanidin B3, procyanidin C2, and/or prodelphinidin B3.

The term "lignan" refers to phenolic compounds formed by two monolignol units. In particular, seicoisoclericiresinol is one of the lignans present in barley.

Phenolic acids include hydroxybenzoic acids and hydroxycinnamic acids.

Hydroxybenzoic acids include gallic acid, syringic acid, vanillic acid, protocatechuic acid, and p-hydroxybenzoic acid.

The term "hydroxycinnamic amino acid" or "coumaric acid" refers to a compound derived from cinnamic acid with a C6-C3 base structure.

Hydroxycinnamic acids include ferulic acids, caffeic acids, sinapic acids, o-coumaric acid, or p-coumaric acid.

Hordatines are secondary plant compounds, particularly found in barley, and therefore also found in malt and barley malt rootlets, with antifungal properties. These molecules belong to the group of phenolamides, which comprise a phenolic nucleus coupled to an amide.

Hordatine A, Hordatine B, Hordatine B1, Hordatine C, Hordatine hexoside, Hordatine hexoside B, Hordatine hexoside B1, Hordatine hexoside C, Coumaroyl hydroxyagmatine and Feruloyl hydroxyagmatine are compounds naturally occurring in barley with antifungal properties.

Hordenine is an alkaloid of the phenylethylamine family comprising a phenolic nucleus and an amide, naturally present in barley, and exhibiting antimicrobial and antifungal properties.

Process

Starting material: the rootlet comprises between 20% and 40% proteins, between 15% and 20% hemicellulose, between 6% and 10% cellulose, between 5% and 10% minerals (notably phosphorus and potassium), between 1% and 3% lipids, vitamins A, B and D.

Depending on the characteristics of the composition to be extracted, the primary consideration may be the protein, lipid, mineral and/or vitamin content. Among the proteins are hordenines, hordatines and associated compounds.

The rootlet contains amino acids, including aspartic acid and glutamic acid, and glutamine groups.

The extraction process involves different steps to extract, purify and concentrate the active ingredients contained in the starting material.

The major steps are:

• La mise en œuvre dans un solvant approprié,

- l’étape d’extraction proprement dite dans laquelle on va soutirer les molécules d’intérêts contenues dans la matière végétale,– Preparation of the material,

• Implementation in a suitable solvent,

- the extraction stage itself in which the molecules of interest contained in the plant material are extracted,

- possible post-processing steps for a composition dedicated to a particular application.

The different steps are detailed below.

Cleaning: If necessary, the raw material is cleaned to reduce the impurity content. Cleaning also separates the rootlets from other barley debris resulting from the separation process, such as broken or whole grains or husks, which allows the subsequent process to be applied to a raw material that is sized, both mechanically and biologically. Cleaning includes, for example, suitable sieving to retain rootlet fragments below a predetermined size threshold, for example, below 2.5 millimeters (mm), in particular below 2 mm, in particular below 0.5 mm, or even below 0.25 mm. However, such sieving is not necessarily necessary, especially if the rootlet fragments resulting from the separation process from the grain are already of a suitable size. Alternatively, densitometric separation is used.

The raw material resulting from this cleaning step is called "screened rootlet". The manufacturing process which is the subject of the present invention is applied to this screened rootlet, or to the rootlet obtained by one or more mechanical treatments (crushing and/or selection) applied to this screened rootlet, as described herein.

Grinding : The sieved rootlet can be ground. At the end of this step, the raw material is modified, such as its particle size distribution, density, appearance, flowability and its use in subsequent processes.

Selection : A fraction of the ground material obtained in the previous step can be selected. This involves selecting a fraction of the ground material defined by a particle size range of particular interest for the rest of the process. For example, a fraction of the ground material with a particle size between L1 and L2 is selected. L2 is greater than L1. L1 is, for example, equal to 0, between 100 and 200 microns, between 100 and 300 microns, between 100 and 400 microns, between 200 and 300 microns, between 200 and 400 microns, between 300 and 400 microns. L2 is for example between 100 and 200 microns, between 100 and 300 microns, between 100 and 400 microns, between 100 and 500 microns, between 100 and 1000 microns, between 200 and 300 microns, between 200 and 400 microns, between 200 and 500 microns, between 200 and 1000 microns, between 300 and 400 microns, between 300 and 500 microns, between 300 and 1000 microns, between 400 and 500 microns, between 400 and 1000 microns, or between 500 and 1000 microns. A ground sieved rootlet of fraction L1-L2 is then obtained.

This selection step includes, for example, one or more sieving operations. However, in the context of the invention, the term "sieved rootlet" refers to that resulting from the initial cleaning step presented above. This selection step can also be densitometric using fluidized bed technology, for example by combining vibrating and pneumatic technologies to create the separation process.

Alternatively, where the grinding operation is not carried out, the selection step can be carried out on the sieved rootlet. A sieved rootlet of fraction L1-L2 is then obtained.

The fraction corresponding to the molecules of interest to be extracted is selected. For example, the fraction below 500 microns is selected for protein extraction. For example, the fraction above 250 microns, or above 500 microns, is selected for the extraction of molecules of interest contained in the fibrous fraction.

The composition of the selected rootlet grinds may differ from the composition of the sieved rootlet. The rootlet grind may contain between 15% and 45% hemicellulose, between 5% and 35% cellulose, and between 1% and 6% lignin. This composition may depend in particular on the particle size range of the grind retained.

The ground material may include glutamine, asparagine, proline, alanine, valine and/or aspartic acid. These amino acids may be included in ground material with particle sizes between 0.125 and 0.5 mm. However, using the entire portion eliminates the need for a selection step. The ground material may contain no more than traces of tyrosine, methionine and/or phenylalanine. The amino acid composition and their presence in the different fractions and the extraction process parameters may be selected to optimize the extraction according to the intended purpose.

Sterilization: A sterilization step is implemented to lower the microbial load of the material, and therefore increase its microbiological quality, while preserving the molecules of interest. Sterilization is, for example, implemented in an autoclave under suitable temperature and pressure conditions. For example, the enclosure is maintained at a suitable temperature, typically above 100°C, in particular above 105°C, 115°C, or even 121°C. The enclosure is maintained at overpressure, at a pressure at least equal to 1 bar, typically above 1.5 bars, or even above 2 bars. Sterilization is, for example, implemented for a sufficient duration, above a predetermined threshold (residence time), for example, above 20 minutes (min), for example, above 30 minutes. Sterilization is also a gentle sterilization allowing the molecules of interest to be preserved. In particular, the temperature can be lower than 125°C, lower than 120°C, or even lower than 110°C. The pressure can be lower than 3 bars, in particular lower than 2.7 bars, lower than 2.2 bars, or even lower than 1.7 bars. The duration can be less than 1 hour, less than 45 minutes, less than 35 minutes, or even less than 25 minutes. The temperature, pressure and duration conditions can be defined according to the raw material, for example following a calibration or calibration.

The sterilization step is designed to avoid impacting the grain size, density, protein, fiber, and/or dry matter content of the raw material. Where applicable, the step may impact the color of the raw material, without impacting the above parameters.

Sterilized ground material has a dry matter ratio of approximately 94 to 96%, a protein to dry matter ratio of approximately 38 to 40%, and a density of approximately 0.43 to 0.45. Particles larger than 0.5 mm are less than 1% by mass. Particles between 0.315 and 0.5 mm are between 38% and 44% by mass. Particles between 0.250 and 0.315 mm are between 23% and 31% by mass. Particles between 0.125 and 0.250 mm are between 25% and 28% by mass. Particles smaller than 0.125 mm are between 4% and 6% by mass.

The sterilization step is designed to drastically reduce the microbial load of the raw material, without degrading the molecules of interest. The raw material before sterilization may contain at least 25 million CFU of presumed coliforms at 30°C per gram. The raw material before sterilization may contain at least 100 million CFU of microorganisms at 30°C per gram. The raw material before sterilization may contain at least 100,000 CFU of mesophilic lactic acid bacteria per gram. The raw material before sterilization may contain at least 10,000 CFU of yeasts (counted after 5 days) per gram. The raw material before sterilization may contain at least 1,000 CFU of molds (counted after 5 days) per gram.

The following table shows the microbiology of the products obtained after sterilization. Coagulase-positive staphylococci at 37°C Colony Forming Units per gram (CFU/g) < 10 E. coli Beta glucuronidase CFU/g < 10 Presumed coliforms at 30°C CFU/g < 1000 Sulfite-reducing anaerobic bacteria 46°C / 25 g < 10 Microorganisms at 30°C (total flora) CFU/g < 1000 Mesophilic lactic acid bacteria CFU/g < 100 Yeasts (Count after 5 days) CFU/g < 100 Molds (Count after 5 days) CFU/g < 100 Bacillus Cereus presumptive) 30°C CFU/g < 10

[Table 2: Microbiology]

Extraction: The extraction step includes a preparation step, a chemical hydrolysis step, and subsequent processing steps.

During the preparation, the sterilized ground material presented above is mixed in an aqueous solvent, in quantities of the order of 1/10 by mass (1 gram of ground material for 10 grams of solvent). According to a first example, the aqueous solvent is a non-alcoholic solvent. It only comprises water. Alternatively, however, the solvent can be alcoholic or hydroalcoholic.

The aqueous solvent is, for example, acidic. For example, the pH of the composition is between 1 and 5, more particularly between 2 and 4, especially between 2.5 and 3.5. For example, citric acid is used, in quantities of the order of 1/10 by mass (1 gram of acid for 10 grams of ground material), mixed with the other components of the solvent before or after mixing with the raw material. Alternatively, lactic, acetic, tartaric, malic and/or sulfuric, or even hydrochloric, acids can be used.

The extraction is for example assisted by microwaves in a suitable container. The microwaves are for example emitted at a frequency of 915 MHz for 60 minutes, with stirring at 70 revolutions per minute, in a material/solvent ratio of 1/10, at a power less than or equal to 100 kW, in particular less than or equal to 80 kW, less than or equal to 50 kW, less than or equal to 20 kW, less than or equal to 10 kW, or even less than or equal to 1 kW. Alternatively, microwaves at 2.450 GHz are used, at a power less than or equal to 25 kW, in particular less than or equal to 10 kW, typically less than or equal to 3 kW, or even less than or equal to 1 kW. Alternatively, a different material/solvent ratio is used, for example between 1/50 and 1/5, in particular between 1/20 and 1/8. Alternatively, the extraction time could be greater than 15 minutes and/or less than 120 minutes. The extraction time is adapted according to the other extraction parameters and their impact on the degradation of the molecules of interest. It is, for example, determined during calibration. The material/solvent ratio, the particle size dispersion of the raw material and the agitation are determined together to promote the transmission of microwaves in the solvent and the achievement of a uniform temperature at the heart of the product. Microwave-assisted technology makes it possible to break the plant walls and access the cellular contents. The microwaves act on the water molecules, which absorb them and release them in the form of heat. The pressure generated homogeneously in the device causes an expansion of the cell walls, thus releasing the intrinsic compounds of the plant cells.

During this extraction, antioxidants present in the raw material are extracted, as listed above, such as flavonoids, coumarins, anthocyanins and/or lignans. These compounds are considered for cosmetic applications.

Subsequent steps may include one or more liquid and solid phase separations, for example by pressing with a filtration size of 100 micrometers, followed by filtration at 25 microns, generating a sufficiently pure liquid extract. These subsequent steps may further increase the extraction yield. The resulting liquid extract is, for example, approximately 7.644 kg and comprises 3.8% dry matter. This liquid extract then comprises the molecules of interest, and may then be post-treated by further steps, such as, for example, concentration at 50°C and 30 mbar. The resulting concentrated liquid extract is, for example, approximately 1.707 kg and comprises 16.99% dry matter. This concentrated liquid extract may further be post-treated by further steps, such as, for example, filtration at 0.14 microns. The resulting filtered concentrated liquid extract is, for example, approximately 591 g and comprises 12.49% dry matter.

The final material comprises amino acids, hydroxycinnamic acids, hordatine hexosides (B1, B, C) and/or hordatines (B1, B, A), ferulolhydroxyagmatine, and/or coumaroylhydroxyagmatine.

The final material includes phenylethylamines, such as hordenines.

The final material may also include betaines, sucrose, chelidonic acid (alkaloid, antioxidant and anti-inflammatory, applicable against headaches or joint pain), malic acid, citric acid, hydroxyoctanoic acid derivatives, lipophosphatidylethanolamines, lipophosphatidylcholines.

The antioxidant activity of a malt-derived composition is higher than that of a barley-derived composition, due to the chemical processes occurring during the malting process, in particular the synthesis of enzymes linked to the germination of the barley grain, leading to a degradation of polymers, the release of phenolic compounds linked to lignin and arabinoxylans, and/or Maillard reactions. The kilning temperature weakens the structure of the molecules and allows for better extraction of phenolic acids.

Example 1

Comparative example

According to a comparative example, a hydro-ethanolic chemical extraction is carried out in the laboratory without microwaves on the two raw materials, sterilized or not, as presented below. Sterilization temperature (°C) Matter Plant walls (g) Hemicellulose (g) Cellulose (g) Lignin (g) Dry matter (%) Protein (% of dry matter) Non-sterile Sifted rootlets 64,660 45,820 12,783 2,823 95.47 38.36 115 Sifted rootlets 68,480 46,350 10,303 4,157 95.26 39.17 Non-sterile Crushed 60,723 40,177 12,350 3,093 94.54 38.54 115 Broyat 61,920 40,230 10,413 4,200 92.92 37.87 Non-sterile Fraction 125 µm-315 µm 56,063 33,200 10,427 4,947 95.55 35.98 115 Fraction 125 µm-315 µm 60,157 37,670 8,657 6,910 93.58 36.40

[Table 3]: Composition of materials before and after sterilization

In this comparative example, applied to 50 grams (g) of raw material, an extraction is carried out at a ratio of 1/18 in an ethanol (70%) – water (30%) solvent for 30 minutes, at 70°C, with stirring (500 rpm). At the end of the extraction, 25 micron filtration, concentration and lyophilization are applied. The corresponding sample is referenced “344-2-1-LYO” for the unground raw material, and “344-3-1-LYO” for the ground raw material. The extraction yield, defined as the mass of the liquid extract multiplied by the dry matter content in the liquid extract, and divided by the mass of raw material, is measured. The mass of the hordatin compounds, coumaroyl hydroxyagmatine, feruloyl hydroxyagmatine and hordenine in the extract is measured. Extraction yield % hordatins A, B, C + hordatins hexoside % coumaroyl hydroxyagmatine % feruloyl hydroxyagmatine % hordenine 344-2-1-LYO 17.20% 0.92 0.25 0.11 0.14 344-3-1-LYO 17.88% 0.95 0.21 0.10 0.14

[ Table 4 ] :Test results

The quantities of active compounds are given as a percentage of the mass of the extracted freeze-dried material.

Example 2

In a second step, a microwave-assisted extraction was carried out, as presented, in aqueous solvent at neutral pH on the sterilized ground material. The yield obtained from the extraction, for the sample referenced "1", was measured at 17.11%. Surprisingly, it was found that microwave-assisted extraction made it possible to obtain yields comparable to hydro-alcoholic extraction. The process implemented has the advantage of avoiding the harmfulness of certain solvents.

Example 3

Thirdly, different protocols were tested in order to evaluate the best in terms of extraction yield and composition of molecules of interest. For all protocols, microwave technology was implemented, as presented above, in order to promote the extraction of these molecules.

The microwave extraction process was carried out in basic (Ref. 3), acid (Ref. 2) or neutral (Ref. 1, already presented above) phase, depending on the characteristics presented. The extraction yield is given in Table 5 below. Ref MP mass engaged (g) Dry MP mass (g) Mass of reactant (g) Water (g) pH Extraction yield in MS (g) 385-2-1-LYO 750 732.90 75 7500 3 22.94% 385-3-1-LYO 750 732.90 50 7500 9 17.32% 385-1-1-LYO 750 732.90 7500 7 17.11%

[ Table 5 ] : Microwave-assisted extraction test results at different pH

In the case of extraction in an acidic or basic medium, the extraction yield is defined as the mass of the liquid extract multiplied by the dry matter content in the liquid extract, and divided by the sum of the mass of raw material and the mass of reagent.

Surprisingly, it turned out that the acid phase extraction process gave a yield much higher than that of the processes implemented in neutral and basic phases.

The amounts of the compounds listed above for the lyophilized extract are measured, related to the mass of lyophilized raw material, and the measurement results are presented in Table 6 below. Ref % hordatins A, B, C + hordatins hexoside % coumaroyl hydroxyagmatine % feruloyl hydroxyagmatine % hordenine 385-2-1-LYO 0.670 0.090 0.040 0.050 385-3-1-LYO 0.090 0.040 0.020 0.040 385-1-1-LYO 0.410 0.100 0.030 0.070

[ Table 6 ] : Test results (percentage in grams per 100 g of freeze-dried rootlet extract)

The amounts of the compounds listed above for the lyophilized extract are measured, reported to the mass of raw material, and the measurement results are presented in Table 7 below. Ref % hordatins A, B, C + hordatins hexoside % coumaroyl hydroxyagmatine % feruloyl hydroxyagmatine % hordenine 385-2-1-LYO 0.169 0.023 0.010 0.013 385-3-1-LYO 0.017 0.007 0.004 0.007 385-1-1-LYO 0.070 0.017 0.005 0.012

[ Table 7 ] : Test results (percentage in grams per 100 g of rootlet)

These results are compared to those from the ethanolic extraction process without microwaves at neutral pH (sample “344-3-1-LYO”) in Table 8 below. Ref % hordatins A, B, C + hordatins hexoside % coumaroyl hydroxyagmatine % feruloyl hydroxyagmatine % hordenine 385-2-1-LYO 0.169 0.023 0.010 0.013 344-3-1-LYO 0.170 0.038 0.018 0.025

[ Table 8 ] : Test results (percentage in grams per 100 g of rootlet) compared with sample 344-3-1-LYO extracted by conventional ethanol extraction.

Surprisingly, it is found that microwave-assisted extraction in the acid phase gives better production yields of each of the compounds studied.

Alternatively, if necessary, a hydro-alcoholic extraction step, in particular hydro-ethanolic, can be implemented following the microwave extraction step in an acid medium. The quantity of alcohol is, for example, between 10% and 80% of the total mass of the composition undergoing extraction. According to one example, an experiment is carried out (sample “385-5-1-LYO”) by carrying out a microwave-assisted extraction in 5,250 g of water, followed by a hydro-alcoholic extraction by adding 2,250 g of ethanol, the rest of the process being unchanged. The extraction yield is given in Table 9 below. Ref MP mass engaged (g) Dry MP mass (g) Ethanol (g) Water (g) Extraction yield in MS (g) 385-5-1-LYO 750 732.90 2250 5250 17.44% 385-1-1-LYO 750 732.90 7500 17.11%

[Table 9 ]: Test results of microwave-assisted extraction followed by hydroalcoholic extraction

Claims (15)

Method of manufacturing a composition comprising:
- we provide malt rootlets,
- an extract is obtained by microwave-assisted extraction of malt rootlets dispersed in a solvent. A method of manufacturing a composition according to claim 1, wherein the malt is a malt of barley, wheat, rye, spelt, corn, millet, sorghum, oats, triticale or rice, in particular a barley malt. A method of manufacturing a composition according to claim 1 or 2, wherein the composition obtained comprises polyphenols,
- in particular flavonoids, more particularly flavonols, flavanols, isoflavones, flavones, flavanones and/or anthocyanins; or polymers thereof, in particular proanthocyanidols;
- and/or in particular non-flavonoids, more particularly curcuminoids, lignans, phenolic acids and/or stilbenes. A method of manufacturing a composition according to claim 3, wherein the composition obtained comprises quercetins, kaempferols and/or catechins; and/or condensed tannins, such as procyanidins and/or prodelphinidins. Process for manufacturing a composition according to one of claims 1 to 4, in which the composition obtained comprises hydroxybenzoic and/or hydroxycinnamic amino acids, in particular ferulic acid, caffeic acid, sinapic acid, o-coumaric acid and/or p-coumaric acid. Process for manufacturing a composition according to any one of claims 1 to 5, in which the composition obtained comprises at least one and/or the other of the following compounds:
- phenolamides, such as for example hordatines, in particular hordatine A, hordatine B, and more particularly hordatine B1, hordatine C and/or hordatine hexoside, and more particularly hexoside B and/or hexoside B1,
- coumaroyl hydroxyagmatine,
- feruloyl hydroxyagmatine,
- phenylethylamine, especially alkaloid, in particular hordenine. A method of manufacturing a composition according to any one of claims 1 to 6, in which the solvent is water, alcohol, or is hydroalcoholic. Process for manufacturing a composition according to any one of claims 1 to 7, in which the solvent is acidic and has a pH preferably between 1 and 5, in particular between 2 and 4, more particularly between 2.5 and 3.5. Manufacturing method according to any one of claims 1 to 8, wherein:
- microwaves are emitted at a frequency of 915 MHz at a power of between 1 and 100 kW; or
- microwaves are emitted at a frequency of 2,450 MHz at a power of between 1 and 25 kW. Method for manufacturing a composition according to any one of claims 1 to 9, in which, before carrying out the extraction, a selection of a fraction of the rootlets is carried out according to their dimensions and/or their density. A method of manufacturing a composition according to any one of claims 1 to 10, in which a hydroalcoholic extraction is further carried out after the microwave-assisted extraction. A method of manufacturing a composition according to any one of claims 1 to 11, in which sterilization, in particular gentle sterilization, is carried out before microwave-assisted extraction. Manufacturing method according to any one of claims 1 to 12, in which a post-treatment of the extract obtained is also carried out. Manufacturing process according to any one of claims 1 to 13, in which the malt rootlets are provided in the form of ground material and/or a ground material fraction. Manufacturing method according to any one of claims 1 to 14, in which, before providing the rootlet, the raw material is cleaned, said cleaning involving at least one sieving and/or one densitometric separation.