WO2014072282A1 - Récupération de caféine et de fraction bioactive de café - Google Patents

Récupération de caféine et de fraction bioactive de café Download PDF

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Publication number
WO2014072282A1
WO2014072282A1 PCT/EP2013/073032 EP2013073032W WO2014072282A1 WO 2014072282 A1 WO2014072282 A1 WO 2014072282A1 EP 2013073032 W EP2013073032 W EP 2013073032W WO 2014072282 A1 WO2014072282 A1 WO 2014072282A1
Authority
WO
WIPO (PCT)
Prior art keywords
caffeine
fraction
coffee
adsorbent
aqueous solution
Prior art date
Application number
PCT/EP2013/073032
Other languages
English (en)
Inventor
Frederico Mora
Johanna Hendrika Schoonman
Thierry Labrunie
Original Assignee
Nestec S.A.
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 Nestec S.A. filed Critical Nestec S.A.
Publication of WO2014072282A1 publication Critical patent/WO2014072282A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F5/00—Coffee; Coffee substitutes; Preparations thereof
    • A23F5/20—Reducing or removing alkaloid content; Preparations produced thereby; Extracts or infusions thereof
    • A23F5/208—Reducing or removing alkaloid content; Preparations produced thereby; Extracts or infusions thereof by extraction of the beans with water, aqueous solutions without organic or inorganic solvents, or aqueous coffee extract
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F5/00—Coffee; Coffee substitutes; Preparations thereof
    • A23F5/20—Reducing or removing alkaloid content; Preparations produced thereby; Extracts or infusions thereof
    • A23F5/22—Reducing or removing alkaloid content from coffee extract
    • A23F5/223—Reducing or removing alkaloid content from coffee extract using flocculating, precipitating, adsorbing or complex-forming agents, or ion-exchangers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52—Adding ingredients
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • 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)
    • A61K36/74—Rubiaceae (Madder family)
    • 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

Definitions

  • the present invention relates to a process of recovering caffeine and bioactive compounds from coffee by adsorbing caffeine and bioactive compounds on an adsorbent following by desorption and collection of at least two fractions of the desorbed material.
  • Coffee beans are rich in many substances with biological effects, e.g. caffeine and polyphenols, such as chlorogenic acids and their lactones, some of which may act as antioxidants. Many of these bioactive compounds are extracted during normal extraction of coffee with water and may exert biological effects in individuals consuming the resulting coffee brew. In some occasions, and by some consumers, the effect of caffeine is not desired, and to satisfy such consumers decaffeinated coffee products, coffee products wherein the content of caffeine has been removed, totally or in part, are produced. Several methods exist for the removal of caffeine from coffee beans. The caffeine removed may be used as an ingredient e.g. in other beverage and/or food products. Caffeine may e.g.
  • WO 2011/011418 discloses a crude caffeine complex obtained as the un-purified complex of caffeine and other compounds remaining after removal of caffeine from coffee beans, and the use of such a crude complex as an ingredient.
  • some of the compounds of the crude caffeine complex may have different benefits and used than others, so a fractionation may be needed or desired. It may especially be desirable to be able to separate the group of polyphenols, which have antioxidant effects, and caffeine, which has stimulating effects.
  • polyphenols e.g.
  • the compounds adsorbed by an adsorbent used for decaffeination of an aqueous extract of coffee beans, apart from caffeine, comprises polyphenols which may be useful as an ingredient, e.g. in food and beverage products. Furthermore, they have found that adsorbed compounds from the decaffeination process can be desorbed with an aqueous liquid, and that polyphenols are desorbed faster than caffeine, so that a first polyphenol rich fraction may be collected, followed by a second caffeine rich fraction. In this way a simple and cost efficient fractionation of the adsorbed compounds may be achieved by desorbing the adsorbed material with an aqueous liquid, and collecting at least two fractions, a first fraction and a second fraction.
  • the invention relates to a method of recovering bioactive compounds and caffeine from coffee, the method comprising: a) extracting coffee beans with an aqueous liquid to obtain an aqueous extract of coffee; b) contacting the aqueous extract of coffee obtained in step a) with an adsorbent to adsorb caffeine and bioactive compounds; and c) recovering adsorbed compounds from the adsorbent of step b) by contacting the adsorbent with an aqueous solution, and collecting a first fraction of the aqueous solution, the first fraction being rich in polyphenols, followed by collecting a second fraction of the aqueous solution, the second fraction being rich in caffeine.
  • Figure 1 shows the cumulated caffeine (total amount of caffeine in the total amount of aqueous liquid used for desorption) over time (dark line) and the cumulated solids (including caffeine and polyphenols) over time for the 1000L scale (light line) for the experiments reported in example 1.
  • Figure 2 shows the cumulated caffeine over time (dark line) and the cumulated solids (including caffeine and polyphenols) over time for the 3L scale (light line) fro the experiments reported in example 1.
  • Coffee beans are extracted with an aqueous liquid.
  • Coffee beans may be the beans from any coffee plant (Coffea), e.g. Arabica coffee (Coffea arabica), and/or Robusta coffee (Coffea canephora).
  • the coffee beans may be green (raw) or roasted, or may have been subjected to any other suitable treatment, e.g. a heat treatment as disclosed in WO 2011/073052.
  • the coffee beans are green coffee beans.
  • the coffee beans may be whole or ground, the coffee beans are preferably whole beans.
  • the extraction may preferably from part fo a process for decaffeination of coffee beans, such as e.g. the process disclosed in US patent No. 5,208,056.
  • the aqueous liquid may e.g. be water or an extract of coffee beans. If an extract of coffee beans is used, the concentration of coffee solids, except caffeine, may preferably be so high that substantially only caffeine is removed from the coffee beans.
  • the aqueous solution used to extract the coffee beans is an aqueous extract of coffee from which caffeine has been removed.
  • the coffee beans may for example be extracted in an aqueous liquid which is re-circulated until it is saturated with coffee solids. During the recirculation the coffee extract may be contacted with an adsorbent to remove caffeine.
  • the coffee extract is contacted with an adsorbent to adsorb caffeine and other bioactive compounds.
  • the adsorbent may be any suitable adsorbent, such as e.g. activated char coal, activated alumina, silica gel, clay minerals, zeolites or a polymer resin such as a molecularly imprinted polymer.
  • the adsorbent may have been loaded with coffee solids other than caffeine to reduce the amount of non-caffeine solids removed from the coffee extracts, e.g. by contacting the adsorbent with a caffeine free coffee extract. In this case, the adsorbent may only adsorb minor amounts of bioactive compounds other than caffeine.
  • Adsorbed compounds are recovered from the adsorbent by contacting the adsorbent with an aqueous liquid.
  • the aqueous liquid is preferably water, but may also contain compounds such as weak protic acids, and halogenated and non-halo genated organic solvents.
  • water is meant water that is substantially free of other components, especially organic solvents such as e.g. ethanol.
  • the contacting may be done as a batch operation or as a continuous operation where used aqueous liquid is continuously collected and new aqueous liquid is supplied, the aqueous liquid may be circulated over the adsorbent and any other suitable way of contacting may be used.
  • the contacting may be performed at any suitable temperature, e.g.
  • aqueous liquid preferably water
  • polyphenols are desorbed faster than caffeine.
  • aqueous liquid preferably water
  • fractions of aqueous liquid collected early in the desorption process will be rich in polyphenols as compared to fractions collected later, which will be relatively rich in caffeine.
  • rich in polyphenols or rich in caffeine is meant that a fraction comprises a higher ratio of polyphenols or caffeine, respectively, out of the total solids in the fraction, as compared to the ratio of polyphenols or caffeine, respectively, in the total of the adsorbed solids.
  • a first fraction of the aqueous solution is collected, the first fraction being rich in polyphenols, followed by collection of a second fraction of the aqueous solution, the second fraction being rich in caffeine.
  • desorption of specific compounds of interest e.g. caffeine or polyphenols
  • concentration of the compound(s) of interest e.g. the concentration in percent of total solids desorbed.
  • the period of collection of each fraction may thus be controlled based on the desorption pattern of each fraction.
  • the process of the invention is not restricted to the collection of a first and second fraction, only. As many fractions as desired may be collected, e.g. depending on the intended use and required composition and purity of compounds, as well as the desired degree of recovery of specific compounds.
  • the collection of the first fraction of the aqueous solution is terminated before the concentration of caffeine in the total amount of aqueous solution used for desorption has reached 40% by weight of total dry matter, such as before the concentration of caffeine in the total amount of aqueous solution used for desorption has reached 50%> more preferably 60%>, by weight of total cumulated dry matter.
  • the collection of the second fraction of the aqueous solution is started after the concentration of caffeine in the total amount of aqueous solution used for desorption has reached 40%> by weight of dry matter, such as the concentration of caffeine in the total amount of aqueous solution used for desorption has reached 50%>, more preferably 60%>, by weight of cumulated dry matter.
  • the collection of the first fraction is terminated before the cumulated amount of caffeine in the first fraction has reached 50% by weight of total cumulated dry matter.
  • the collected fractions may be subjected to any subsequent treatments suitable for their intended use. They may e.g. be concentrated, e.g. by removing water, e.g. with evaporation or filtration, and they may be subjected to further purification steps to further purify and/or separate specific compounds or groups of compounds.
  • the collected fractions may also be dried.
  • the method of the invention comprises drying the first fraction rich in bioactive compounds obtained in step c), or part of this fraction, to produce a dry composition of bioactive compounds.
  • the method of the invention comprises drying the second fraction rich in caffeine obtained in step c), or part of this fraction, to produce a dry preparation of caffeine.
  • the bioactive compounds and the caffeine obtained by the method of the invention may have many uses, e.g. as ingredients of food supplements, food products, beverage products, pet food products, skin care products, medical products, and medical food and beverage products.
  • the method of the invention further comprises using the first fraction obtained in step c) as an ingredient of a food supplement, a food product, a pet food product, or a beverage product.
  • Suitable beverage products are e.g. coffee products, such as e.g. soluble coffee, and roast and ground coffee, e.g. roast and ground coffee in capsules; cocoa beverages; malt beverages; fruit or vegetable juice based beverages; and milk based beverages.
  • Suitable food products are e.g. confectionary products, e.g. chocolate products; sports nutritional products, e.g. energy bars; infant nutrition products;
  • a green coffee extract of total solid content 5% (TC: mass of matter in a coffee solution defined as the weight (w) of the dried coffee residue expressed as a percentage of the original coffee solution or suspension in weight/weight percent (w/w%)) and caffeine concentration of 0.5 (w/w%) was contacted with a fixed volume of active carbon (3L and 1000L) for lOhr. After this contacting, the non adsorbed coffee extract was displaced with 1 bed volume of water. The active carbon was then washed with water at 150°C for 24h to recover the adsorbed solids. The concentration of caffeine and the concentration of total solids were monitored throughout the experiment.
  • Figure 1 shows the cumulated caffeine (total amount of caffeine in the total amount of aqueous liquid used for desorption) over time (dark line) and the cumulated solids (including caffeine and polyphenols) over time for the 1000L scale (light line). It is to note that 10 sets of experiments were performed and for clarity only one figure is used.
  • Figure 2 shows the cumulated caffeine over time (dark line) and the cumulated solids (including caffeine and polyphenols) over time for the 3L scale (light line). It is to note that 10 sets of experiments were performed and for clarity only one figure is used.

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Botany (AREA)
  • Mycology (AREA)
  • Nutrition Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Tea And Coffee (AREA)

Abstract

La présente invention concerne un procédé pour récupérer la caféine et les composés bioactifs du café par mise en contact d'un extrait de café avec un adsorbant pour adsorber la caféine et les composés bioactifs et récupération ultérieure des composés adsorbés par mise en contact de l'adsorbant avec un liquide aqueux et recueil d'au moins deux fractions du liquide aqueux.
PCT/EP2013/073032 2012-11-08 2013-11-05 Récupération de caféine et de fraction bioactive de café WO2014072282A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP12191826 2012-11-08
EP12191826.2 2012-11-08

Publications (1)

Publication Number Publication Date
WO2014072282A1 true WO2014072282A1 (fr) 2014-05-15

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017060215A1 (fr) 2015-10-09 2017-04-13 Nestec S.A. Procédé de micronisation de particules de café
EP4327666A1 (fr) 2022-08-26 2024-02-28 ANKA Angewandte Kaffeetechnologie GmbH Procédé et dispositif de préparation de grains de café vert décaféinés et de la caféine, utilisant des résines adsorbantes, et utilisations correspondantes

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4160042A (en) * 1977-07-29 1979-07-03 Farr David R Process for treating an aqueous extract of a vegetable material
US4506072A (en) * 1983-04-18 1985-03-19 Hag Gf Aktiengesellschaft Regeneration of caffeine-loaded activated carbon with hot water
US4548827A (en) * 1982-03-30 1985-10-22 General Foods Corporation Separate recovery of caffeine and coffee solids adsorbed on activated carbon
US5208056A (en) 1978-08-22 1993-05-04 Chocolat Suchard Societe Anonyme Process for decaffeinating raw coffee
EP1854780A1 (fr) * 2005-03-01 2007-11-14 Kao Corporation Procede de production d'une composition d'acide chlorogenique
WO2011011418A1 (fr) 2009-07-21 2011-01-27 Kraft Foods Global Brands Llc Complexe de caféine brute, produits alimentaires améliorés utilisant le complexe de caféine brute, et procédés d’utilisation de ceux-ci
WO2011073052A1 (fr) 2009-12-18 2011-06-23 Nestec S.A. Procédé de production d'un extrait de café vert

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4160042A (en) * 1977-07-29 1979-07-03 Farr David R Process for treating an aqueous extract of a vegetable material
US5208056A (en) 1978-08-22 1993-05-04 Chocolat Suchard Societe Anonyme Process for decaffeinating raw coffee
US4548827A (en) * 1982-03-30 1985-10-22 General Foods Corporation Separate recovery of caffeine and coffee solids adsorbed on activated carbon
US4506072A (en) * 1983-04-18 1985-03-19 Hag Gf Aktiengesellschaft Regeneration of caffeine-loaded activated carbon with hot water
EP1854780A1 (fr) * 2005-03-01 2007-11-14 Kao Corporation Procede de production d'une composition d'acide chlorogenique
WO2011011418A1 (fr) 2009-07-21 2011-01-27 Kraft Foods Global Brands Llc Complexe de caféine brute, produits alimentaires améliorés utilisant le complexe de caféine brute, et procédés d’utilisation de ceux-ci
WO2011073052A1 (fr) 2009-12-18 2011-06-23 Nestec S.A. Procédé de production d'un extrait de café vert

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017060215A1 (fr) 2015-10-09 2017-04-13 Nestec S.A. Procédé de micronisation de particules de café
EP4327666A1 (fr) 2022-08-26 2024-02-28 ANKA Angewandte Kaffeetechnologie GmbH Procédé et dispositif de préparation de grains de café vert décaféinés et de la caféine, utilisant des résines adsorbantes, et utilisations correspondantes
WO2024042249A1 (fr) 2022-08-26 2024-02-29 Anka Angewandte Kaffeetechnologie Gmbh Procédé et dispositif de production d'extraits de grains de café brut décaféinés et de caféine à l'aide de résines adsorbantes et de dichlorométhane, et utilisations correspondantes

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