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WO2012031592A1 - Extraction d'hydrocolloïdes à partir de graines de fenugrec (trigonella foenum graecum) - Google Patents

Extraction d'hydrocolloïdes à partir de graines de fenugrec (trigonella foenum graecum) Download PDF

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Publication number
WO2012031592A1
WO2012031592A1 PCT/DK2010/000124 DK2010000124W WO2012031592A1 WO 2012031592 A1 WO2012031592 A1 WO 2012031592A1 DK 2010000124 W DK2010000124 W DK 2010000124W WO 2012031592 A1 WO2012031592 A1 WO 2012031592A1
Authority
WO
WIPO (PCT)
Prior art keywords
salts
solution
extraction
galactomannans
seeds
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/DK2010/000124
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English (en)
Other versions
WO2012031592A8 (fr
Inventor
Ernest Georg Mhlanga
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to PCT/DK2010/000124 priority Critical patent/WO2012031592A1/fr
Publication of WO2012031592A1 publication Critical patent/WO2012031592A1/fr
Anticipated expiration legal-status Critical
Publication of WO2012031592A8 publication Critical patent/WO2012031592A8/fr
Ceased legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/238—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seeds, e.g. locust bean gum or guar gum
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction

Definitions

  • the present invention is concerned with the extraction of valuable substances from plant seeds.
  • this application deals with a novel and economic process for the extraction of the hydrocolloids from fenugreek seed.
  • the fenugreek plant belongs to the leguminous family and is an annual plant.
  • the plant is native to Western Asia and has since spread widely over Asia, Europe, North Africa and the Middle East.
  • hydrocolloids in fenugreek seeds are highly branched galactomannans having a galactose:mannose-ratio of about 1:1, in rare cases about 1:2.
  • the galactomannans present in the mucilage of fenugreek seeds may be
  • extracts from fenugreek seeds are used to provide a dietary supplement.
  • the hydrocolloids are extracted together with proteins from crushed seeds using various solvents and/or aqueous solutions.
  • the seeds are grounded, crushed, milled or otherwise pulverised prior to extraction in order to increase the rate of extraction.
  • a problem associated with the prior art galactomannan extraction processes disclosed or mentioned in the documents cited above is a lack of selectivity whereby other substances than galactomannans are extracted simultaneously, resulting in discoloured, bitter tasting and smelling galactomannan products and cumbersome and costly purification of the galactomannans may be necessary.
  • the invention relates to a method of extracting galactomannans from fenugreek seeds comprising the steps of:
  • said salts being present in an amount of 0.5 - 10% by weight of the solution, adjusting the pH in the solution to be in the range of 1 to 5 with an acid,
  • the galactomannans are released at low temperatures even from whole seeds at an adequate rate. Enzymatic processes normally being triggered by the immersion of the seeds in water are at least partly inhibited by the added salts, whereby e.g. the formation of bitter-tasting substances is diminished and a more neutrally tasting product may be obtained.
  • Discolouration of the galactomannan product by brown colour (probably released from the husk surrounding the seeds) and/or yellow colour (probably released from the cotyledon) may be drastically diminished due to the use of an acidic solution of salts as extraction medium according to embodiments of the present invention
  • the extraction process may be run at comparatively low temperature, thereby selectively extracting the gum from the fenugreek seeds, whereby a substantially pure galactomannan product may be obtained.
  • the salts are selected from the group consisting of sodium salts, potassium salts, calcium salts barium salts, copper salts, magnesium salts, iron salts and any combination thereof.
  • non-toxic salts in the extraction medium. Although the salts are more or less removed when washing the galactomannan product, it may be desirable to use salts that when present in small amounts are unproblematic when using the galactomannans in applications related to food, cosmetics or pharmaceuticals.
  • NaCl, KC1 and/or CaCl 2 are used as salts in the extraction medium.
  • the acid is selected from the group consisting of acetic acid, hydrochloric acid, nitric acid and sulphuric acid.
  • Adjusting the pH to obtain an acidic extraction medium is mandatory according to the present invention. Since the beneficial effects of the acid, e.g. the diminishing of product discolouration, is not dependent on the actual acid used, the acid should be cheap and, preferably, not comprise toxic or otherwise harmful substances.
  • a preferred acid, according to an embodiment of the present invention, is acetic acid.
  • the steps may be regarded as purifying steps, by which the galactomannans are washed so that salts and other residues from the extraction process are removed.
  • the salts from the extraction solution and washing solutions may be recovered and reused.
  • the pH is in the range of 2 - 4, preferably in the range of 2.5 - 3.5.
  • the temperature of the solution is in the range of 20 - 50 °C, preferably in the range of 30 - 40 °C.
  • the extraction process according to the present invention may be run at
  • the extraction method comprises the step of infusing the fenugreek seeds with a solution of one or more salts prior to the step of immersing the fenugreek seeds in the acidic salt-containing solution.
  • the fenugreek seeds When infused with a solution of salts, the fenugreek seeds will swell, but no galactomannans are released from the seeds. Infusion with a solution of salts prior to extraction may speed up the extraction process, whereby the time required at elevated temperatures may be diminished, and thereby further protecting temperature sensitive substances in the fenugreek seeds.
  • Preferred salts for the infusion-solution are selected from the group consisting of sodium salts, potassium salts, calcium salts barium salts, copper salts, magnesium salts, iron salts and any combination thereof.
  • NaCl, KC1 and/or CaCl 2 may be used according to embodiments of the present invention.
  • the fenugreek seeds are used as whole seeds in the extraction.
  • a particular advantage of this embodiment of the present invention is that galactomannans in high yield are selectively being extracted from whole fenugreek seeds, leaving the seeds more or less intact after extraction.
  • the seeds contain valuable oils and other substances that are still comprised in the solid seeds after the gum is extracted when using whole seeds in the extraction process. Further processes to obtain e.g. valuable oils may therefore advantageously be performed on the seed mass after galactomannan extraction.
  • the fenugreek seeds are dry milled prior to extraction.
  • Dry milling crushes the fenugreek seeds, whereby a faster rate of extraction may be obtained due to the larger surface area of the milled seeds when compared to whole seeds.
  • the fenugreek seeds are wet milled prior to extraction.
  • wet milling crushes the fenugreek seeds, whereby a faster rate of extraction may be obtained due to the larger surface area of the milled seeds when compared to whole seeds.
  • the use of a wetting medium may prevents the formation of dust during the milling process.
  • the wetting medium is a solution of one or more salts.
  • the salts in the wetting medium are selected from the group consisting of sodium salts, potassium salts, calcium salts, barium salts, copper salts, magnesium salts, iron salts and any combination thereof.
  • Preferred salts are e.g. NaCl, KC1 and/or CaCl 2 .
  • the infused fenugreek seeds are frozen and thawed prior to extraction.
  • the galactomannans obtained from fenugreek seeds according to the present invention are of high quality and are useful in many applications.
  • the galactomannans obtained according to the disclosed extraction method can be used in basic compositions for food and cosmetics.
  • Examples 2 and 3 are comparative example, the extraction being run at a pH outside the range disclosed in claim 1.
  • the volume of the seeds increases, because the galactomannans in the seeds take up water. Then, the seed coat begins to break and galactomannans are released into the solution. The seed coat and the cotyledons separate. If stirring is too vigorous, the cotyledons will break up.
  • the extraction mixture is sieved, thereby separating the solid parts, retained on the sieve, and the liquid phase containing the desired galactomannans, passing through the sieve.
  • IPA-spirit a blend of 90% ethanol and 10% isopropanol
  • the deposited gum comprising galactomannans is collected with a spoon into a beaker. Most of the liquid that runs out from the gum is drained away.
  • the gum is re-dissolved in clean water and then deposited with a new portion of IPA-spirit.
  • the steps of dissolving and depositing the gum are carried out at least three times in total to obtain a product whiter in appearance and substantially free of salts and acid.
  • the seed mass is washed with 5% salt solution, until all gum is removed from the seeds.
  • the gum product is dried in a hot air oven at 30 - 50 °C for 3 - 8 hours. A yield of 10 g is obtained.
  • the dried galactomannan gum is white, odourless and has a neutral taste.
  • the obtained galactomannans have good solubility in water. Comparative example 2
  • a strong yellow colour is released from the seed into the solution within a few minutes.
  • the released gum becomes yellow as a consequence, and the colour can not be removed in the washing steps.
  • the dried gum product has a yellow colour and slightly bitter taste.
  • the colour intensity diminishes, if during the extraction, the pH is adjusted to about 3 with an acid, but the colour does not disappear completely.
  • the obtained gum product has yellow-brown colour and non-neutral taste.
  • the solution is kept at 40 °C and intermittently slowly stirred.
  • Example 1 After milling the seeds became a powder - this means that all cell content was mixed together and the result was a porridge mixture.
  • the powder was immersed in an extraction medium according to Example 1 and the extraction was performed according to the process of Example 1. To isolate the gum, the solution was passed through a conventional filter but during filtration severe filter blocking was experienced. The gum was deposited according to the procedures in Example 1. The product yield was small and the colour grey, indicating impurities like protein and starches.
  • the solids collected after extraction according to the present invention further contain valuable products that may be obtained through further process steps.
  • valuable products e.g. oils and proteins, may be obtained.
  • Example 4 shows that the extraction process according to the present invention can also be used on milled seeds, in this case, fenugreek seeds subjected to wet milling after infusion in a salt solution overnight.
  • the extraction process becomes more troublesome in that the separation of the solids and the solution containing the extracted gum is not as straightforward as when using whole seeds like in Example 1. Also, because the seeds are destroyed when milled, whereby the whole seed content is subjected to the extraction medium, the gum product obtained is not as pure as when using whole seeds for the extraction.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mycology (AREA)
  • Nutrition Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Botany (AREA)
  • Animal Behavior & Ethology (AREA)
  • Biotechnology (AREA)
  • Dispersion Chemistry (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Alternative & Traditional Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Cosmetics (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

La présente invention concerne un procédé d'extraction de galactomannanes à partir de graines de fenugrec, comprenant les étapes consistant à préparer une solution d'un ou plusieurs sels dans de l'eau, lesdits sels étant présents à hauteur de 0,5 à 10 % en poids de la solution, à ajuster le pH de la solution pour qu'il se situe dans un intervalle de 1 à 5 au moyen d'un acide, à maintenir la température de la solution dans une fourchette de 10 à 60 °C, à plonger les graines de fenugrec dans la solution pendant 2 à 72 heures, à recueillir les galactomannanes présents dans la solution et à récupérer les graines de fenugrec en vue de leur faire subir un autre traitement.
PCT/DK2010/000124 2010-09-06 2010-09-06 Extraction d'hydrocolloïdes à partir de graines de fenugrec (trigonella foenum graecum) Ceased WO2012031592A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/DK2010/000124 WO2012031592A1 (fr) 2010-09-06 2010-09-06 Extraction d'hydrocolloïdes à partir de graines de fenugrec (trigonella foenum graecum)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/DK2010/000124 WO2012031592A1 (fr) 2010-09-06 2010-09-06 Extraction d'hydrocolloïdes à partir de graines de fenugrec (trigonella foenum graecum)

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WO2012031592A1 true WO2012031592A1 (fr) 2012-03-15
WO2012031592A8 WO2012031592A8 (fr) 2013-07-11

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0742007A1 (fr) 1995-05-12 1996-11-13 Laboratoires Serobiologiques Utilisation d'extraits de graines de cassia et/ou de trigonelle enrichis en galactomannanes et produit cosmétique ou pharmaceutique, notamment dermatologique, contenant de tels extraits
EP0775451A1 (fr) 1994-11-24 1997-05-28 Vitamed Remedies Private Limited Produit contenant des fibres alimentaires et procédé pour le préparer
US20010024665A1 (en) 2000-02-14 2001-09-27 Rao Garrimella B. Process for obtaining useful materials from fenugreek seeds
WO2009053652A2 (fr) 2007-10-16 2009-04-30 Bruno Eto Composition pharmaceutique ou dietetique pour inhiber l'absorption intestinale du sucre
WO2009057125A1 (fr) 2007-10-29 2009-05-07 Avesthagen Limited Composition fibreuse alimentaire organoleptiquement améliorée et procédé associé (teestar)

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0775451A1 (fr) 1994-11-24 1997-05-28 Vitamed Remedies Private Limited Produit contenant des fibres alimentaires et procédé pour le préparer
EP0742007A1 (fr) 1995-05-12 1996-11-13 Laboratoires Serobiologiques Utilisation d'extraits de graines de cassia et/ou de trigonelle enrichis en galactomannanes et produit cosmétique ou pharmaceutique, notamment dermatologique, contenant de tels extraits
US20010024665A1 (en) 2000-02-14 2001-09-27 Rao Garrimella B. Process for obtaining useful materials from fenugreek seeds
WO2009053652A2 (fr) 2007-10-16 2009-04-30 Bruno Eto Composition pharmaceutique ou dietetique pour inhiber l'absorption intestinale du sucre
WO2009057125A1 (fr) 2007-10-29 2009-05-07 Avesthagen Limited Composition fibreuse alimentaire organoleptiquement améliorée et procédé associé (teestar)

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Publication number Publication date
WO2012031592A8 (fr) 2013-07-11

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