FR2867686A1 - Production of fenugreek seed oil (I) of Trigonella foenum-graecum, useful in cosmetics, comprises dehulling and crushing the seed, extracting oil from the seed (either by solvent or pressure) and purifying the oil - Google Patents

Abstract

Preparation of fenugreek seed oil (I) of Trigonella foenum-graecum comprising dehulling and crushing the seed, extracting the oil from seed (either by solvent or pressure) and purification of oil, is new. An independent claim is also included for purification of (I) comprising acid demucilagination of the oil (1-5 %) at 60-85 (preferably 75)[deg]C followed by addition of water (2-5 %), agitation and centrifugation; and alkaline neutralization (preferably with soda/sodium hydroxide) of the obtained oil at 60-85 (preferably 75)[deg]C for 30 minutes.

Description

TOURNAY BIOTECHNOLOGIES

The present invention relates to the production of an oil, extracted from fenugreek seed-Trigonella Foenum Graecum-its extraction method, its purification, its composition, its applications for nutrition and cosmetics for the present application. invention.

2] Fenugreek -Trigonella Foenum Graecum- is a butterfly legume, native to Asia Minor, cultivated since antiquity around the Mediterranean basin for the production of fodder and seeds.

3] During dehulling and grinding, the seed is separated into two fractions of different densities, the integument and albumen fraction, which contain a large proportion of mucilage-galactomannan man-and the cotyledon and embryo fraction, comprising almost all the lipids , will be used preferentially for the extraction of the oil.

4] The extraction of the oil can be carried out either by cold or hot pressure, or by solvent extraction, preferably with hexane, or by supercritical fluid with preference for carbon dioxide (CO2), or by any other means known to those skilled in the art.

5] The dehulled seed contains 5 to 10% oil, for the most common seed qualities, without these contents being limiting.

6] Extraction by pressure of the seed or of the cotyledonlembryon fraction at cold (20 to 60 C) or at hot (60 to 80 C) makes it possible to recover 1 to 5% of oil. Extraction with supercritical fluid, preferably CO2, allows the recovery of 6 to 10% of oil. These methods are just as valid as extraction by solvent, preferably hexane. For reasons of cost, the examples given below were made with oils extracted with solvent and then purified; the purification method is valid regardless of the extraction method.

7] Solvent extraction preferentially requires a flattening of the seeds, firstly by crushing between rolls, the spacing being less than 1 mm, the flattening is carried out as extraction takes place to avoid the oxidation of C 18: 3 alphalinolenic acid, the desolvation is carried out by heating the oil with a temperature control at less than 110 C, preferably less than 90 C and greater than 70 C to evaporate hexane or any other solvent. Temperatures mean 1013 mB ordinary pressure; in case of partial evacuation the temperature will be lowered to less than 70 C to ensure perfect evaporation of the solvent.

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8] The purification of the oil is a non-obligatory step, especially for dietetics where the crude oil can be encapsulated directly, but also for cosmetics, for example making soap or perfumed milks. For certain applications, the oil must be purified, freed from its mucilage, its color, some of its odor; the various purification steps are inherent parts of this patent and for all subsequent applications.

9] The purification comprises several steps, which may be non-limiting and depend on the origin of the seed, for example acid degumming, preferably 75% phosphoric acid, added to the oil at a rate of 1 to 5%, a temperature of 60 ° C. or 85 ° C., preferably 75 ° C., and then adding water at a rate of 2 to 5%, followed by stirring and centrifugation.

0] The acid degumming is followed by an alkaline neutralization, preferentially sodium hydroxide sodium hydroxide service temperature will be from 60 to 85 C, preferably 75 C, with a contact time sufficient to neutralize the acid, preferably 30 minutes about.

1] The step following demucilagination is the washing by adding water at a rate of 5 to 20% relative to the amount of oil, with stirring sufficient to wash the product is 5 to 60 minutes, preferably 10 to 15 minutes at a temperature above 50 ° C., preferably 90 ° C., followed by decantation of one night for the first wash and of the order of one hour for the following, the washes being repeated until the oil is neutral. 2 to 6 washes are required.

2] The washing is followed by a discoloration and filtration of the recovered oil, the temperature is between 60 and 110 C, preferably 90 C, so as to make it fluid, the bleaching material is that usually used by man of the art, preferentially the optimum Tonsil 210 FF for example or activated carbon powder, granule, cloth, for example companies PICA or CECA, the amount of filtering earth or activated carbon is of the order of 1 to 5% advantageously 2%.

3] The deodorization step removes part of the fenugreek odor, very characteristic, from a molecule called sotolone, the deodorization time is several hours, preferably 4 hours, at a temperature of 155 C and an injection of 1 to 3% of steam per kg of oil per hour, preferably 1.5%.

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4] The fatty acid composition, after purification, may vary slightly from one seed quality to another, a non-limiting example being provided hereinafter: Polyunsaturated Fatty Acids or PUFA including Omega 6 linoleic acid 40.6% Omega 3 and linolenic alpha 25.3% Total PUFA 65.9% [0015] The fatty acid distribution is as follows Table 1:

Table 1

  Percentage average composition and g content per 100 g of fatty acids Determination of cis and trans isomers FATTY ACIDS COMMON NAMING% 12: 0. a. lauric 0.20 14: 0. a. myristic 0.20 14: 1. a. myristoleic <0.1 16: 0. a. palmitic 13,20 16: 1. a. palmitoleic 0.10 17: 0. a. margaric ND * 17: 1. <0.1 18: 0. a. stearic 3.30 18: 1. a. oleic 12.80 18: 2. a. linoleic 40.60 18: 3. a. linolenic 25.30 20: 0. a. arachidic 1.10 20: 1. at. Gondoque 0.50 22: 0. a. Behenic 0.60 22: 1. a. erucic 0.30 24: 0. a. lignoceric 0.20 24: 1. a. nervonic <0,1 unidentified 1,60

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6] Average total sterol composition Table 2:

Table 2

  Percentage and mg content per 100g total sterols of fenugreek oil% Cholesterol composition 5.70 Brassicasterol 2.80 24 Methyl. Cholesterol 0.50 Campesterol 10.90 Campestanol 0.40 Stigmasterol 0.30 A 7 Campesterol 0.70 A 5.23 Stigmastadienol 1.00 Clerosterol (3 Sitosterol 65.80 Stigmastanol 1.20 A 5 Avenasterol 5.50 A 5, 24 Stigmastadienol 0.70 A 7 Stigmasterol <0.1 A 7 Avenasterol 0.20 Not identified 4.30 Total sterols in mg / 100 g fat 1363

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7] Average Composition in Tocopherols, Tocotrienols Table 3:

Table 3

  Content in mg per kg tocopherols of fenugreek oil Content in mg / 100 g Tocopherols at 590 R 6 Y 24 6 3 Tocotrienols at 3 R <2 y <2 6 <2 Sum 626 Vitamin activity E 59.6 a - TE / 100 g Other non-exhaustive determinations are as follows: Phosphorus determination 216 mg / kg Determination of unsaponifiables 2.5 g / 100 g Lead content 0.26 mg / kg Copper content 0.024 mg / kg Iron 1.776 mg / kg Moisture content 0.05 g / 100 g Insoluble impurity 0.05 g / 100 g Polymerized triglycerides 3.1 to 3.3% Fenugreek oil, semi-drying, is currently known to its incorporation in the manufacture of alkyl resins, recoverable in the paint and varnish industry.

9] Its refining makes it possible, according to the present invention, to use it advantageously in the cosmetics industry and in the nutritional field, with or without additives.

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For example, the oil can be incorporated directly into a soft capsule preferably composed of gelatin and glycerin, as well as coloring additives.

1] The oil may likewise be mixed with preserving or antioxidant agents such as, for example, wheat oil, tocopherols derived from a rosemary extract, or any other natural extract comprising vitamin. E, as well as vitamin E synthesis.

2] The oil can likewise be incorporated in the transparent hard or opaque capsules preferably to avoid the harmful effects of light and the oxidation with or without preserving agents as described in chapter [0021].

3] The fenugreek oil can advantageously be mixed and homogenized at room temperature in a homogenizer at a pressure of 30 to 200 bar so as to form a stable emulsion and be incorporated in a liquid or pasty solution to form a gel, a spray , a lotion, a cream, a shampoo, an ointment, a mousse.

4] Fenugreek oil can be mixed according to techniques known to those skilled in the art to form water-in-oil or oil-in-water emulsions.

5] Fenugreek oil, because of its richness in omega 6 and omega 3 fatty acids, its composition rich in sterols, tocopherols and its vitamin E activity, can advantageously be used in the cosmetic field as a protector, alone or mixed, human keratin skin, hair, nails, anti-UV, protective free radicals caused by fumes, solvents, pollution, protector against drying out, irritation, loss of elasticity, wrinkles the skin.

6] The fenugreek oil, by its composition recalled in paragraph [0021] can advantageously be used in the nutritional field in form, for example, in paragraph [0019] against skin dryness, internal hydration to curb the appearance of signs of age, to help lower cholesterol levels, to curb the oxidation of internal tissues.

7] Fenugreek oil, for its cosmetic or nutritional applications can be used in composition with tensing agents such as hydrolysates of vegetable or animal proteins.

8] Fenugreek oil can also be used in composition with moisturizing agents such ceramides, phospholipids, oligosaccharides and polysaccharides of glucuronic acid, hyaluronic acid, galacturonic acid, chitosan.

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9] Fenugreek oil can also be used in composition with antioxidants such as polyphenols, preferably plant polyphenols such as olive leaf extracts, tea leaves, grape extracts, strawberry, blackcurrant, of bilberry, isoflavones of soybean, clover, stilbene, rutin or quercetin without these extracts being a limiting list.

0] Examples of powdered fenugreek oil preparation for capsule filling in nutritional applications: Use for 70 kg of mixture 33.5 kg of fenugreek oil, 7.1 kg of malto dextrin type DE 18 or Preferred DE 20-, 1.4 kg sodium caseinate or protein hydrolyzate PROT type 24 TOURNAY BIOTECHNOLOGIES- example hydrolysates wheat protein, 28 kg water.

  Put caseinate or PRO 24 in solution in cold or warm water at room temperature, shake to dissolve well, then add malto dextrin, shake for complete dissolution. Then add, with stirring, the fenugreek oil, heat between 30 and 60 ° C., preferably at 45 ° C., homogenize the solution at a pressure of between 50 and 150 bar.

  There is no rise in viscosity, the product remains stable hot or cold. The drying is carried out in a spray tower preferably with a product inlet temperature between 45 and 60 C, a hot air inlet temperature of between 165 and 180 ° C., and an outlet temperature of between 85 and 95 ° C. collected powder, light brown color, has less than 6% moisture; it is not very sticky and not very hygroscopic. It is incorporated as such or in combination with active ingredients such as polyphenols, gums, proteins or amino acids, stilbenes, carotenoids in capsules, dragees, sachets, boxes, tablets, ... for all nutritional needs.

1] Example of a composition intended to produce a stable emulsion for a cosmetic product: 1 Emulsifier type cetearyl olivate / sorbitan olivate 2 to 8% 2 Alkyl ester benzoate type 2 to 6% 3 Fenugreek oil 30 to 50% 4 Water qs 100% Xanthan gum 0.05 to 0.1% Possibility of adding preservatives, perfumes.

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  Method: Mix 1-2-3 at a temperature of 60 to 85 ° C., Mix 4-5 at a temperature of 60 to 85 ° C., stir the phase (1-2-3) to (45) with stirring and lower the temperature. for several hours.

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Claims (12)

  1. Process for producing oil contained in fenugreek seed Trigonella Foenum Graecum its composition and characterization of invention, repeated in chapters [0001] to [0013].   2. Process for the purification of oil contained in the fenugreek seed included in the invention chapters [0008] to [0013].   3. Use of fenugreek oil, raw or purified in that it can be used alone in applications for cosmetics or dietetics.   4. Use of fenugreek oil, purified in that it contains more than 50%, preferably more than 64% of polyunsaturated fatty acids; for cosmetic or dietary applications.   5. Use of fenugreek oil, raw or purified, in that it contains more than 1% total sterols, more than 0.5% tocopherols, and vitamin E activity. 6. Use of fenugreek oil, coming into composition with additives such as antioxidants, tensors, phospholipids, organic acids, polyphenols.   7. Use of fenugreek oil in that it can be incorporated into water-in-oil or oil-in-water emulsions for cosmetic or dietary applications.   8. Use of fenugreek oil in that it may be presented in capsules, flasks, capsules, jars, or any other presentation.   9. Use of fenugreek oil in that it can be mixed and / or homogenized to form liquids, pastes, gels, spray, lotions, creams, foams, ointments.   10. Process for preparing fenugreek oil to form a powder and its uses in dietetics or cosmetics.   11. Use of fenugreek oil, alone or according to the compositions of claims 6 to 10 in that its applications are in the cosmetic field: the protection of keratin skin, hair, nails. TOURNAY BIOTECHNOLOGIES   12. Use of fenugreek oil, alone or according to the compositions of claims 6 to 10 in that its applications are in the nutritional field: internal hydration, skin dryness, lowering of cholesterol and the reduction of internal oxidation.