WO2020086431A1 - Dispositif et procédé d'extraction d'analyte de sélection optimisé - Google Patents

Dispositif et procédé d'extraction d'analyte de sélection optimisé Download PDF

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Publication number
WO2020086431A1
WO2020086431A1 PCT/US2019/057151 US2019057151W WO2020086431A1 WO 2020086431 A1 WO2020086431 A1 WO 2020086431A1 US 2019057151 W US2019057151 W US 2019057151W WO 2020086431 A1 WO2020086431 A1 WO 2020086431A1
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WO
WIPO (PCT)
Prior art keywords
extraction
vessel
solvent
analyte
sonication
Prior art date
Application number
PCT/US2019/057151
Other languages
English (en)
Inventor
James SINKA
Andrew FLEISCHER
Original Assignee
Moonshot Brewing Holdings, Inc.
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 Moonshot Brewing Holdings, Inc. filed Critical Moonshot Brewing Holdings, Inc.
Publication of WO2020086431A1 publication Critical patent/WO2020086431A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00—Tea; Tea substitutes; Preparations thereof
    • A23F3/16—Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • 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
    • A23F5/24—Extraction of coffee; Coffee extracts; Making instant coffee
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0253—Fluidised bed of solid materials
    • B01D11/0257—Fluidised bed of solid materials using mixing mechanisms, e.g. stirrers, jets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • B01D11/0265—Applying ultrasound

Definitions

  • the present invention relates to brewing techniques and devices; and more particularly to analyte extraction techniques and devices; and even more particularly to analyte extraction techniques and devices for extracting bioavailable compounds from plants.
  • Cold Brew coffee and tea (“cold brew”) has become a popular drink. This rise in popularity is due in part to the lowered concentration of unwanted compounds produced through the cold brewing process (i.e., brewing with water temperatures at or below room temperature (about 20°C)) as opposed to hot brewing which uses water temperatures in the range of about 70°C to l00°C. Fewer unwanted compounds enhances the beverage experience.
  • a second downside is that the higher temperature of the solvent (water) causes more collisions at a high energy state (due to the high temperature of the environment) to occur, between the compounds in the solvent. These high frequency collisions at high thermal energies increase the statistical likelihood, and provide the right chemical energy for, reactions to occur between the compounds in the solvent. Similar to most organic chemistry reactions, increasing the temperature increases the rate of the reaction in a hot brew. Furthermore, increasing the temperature enables the proper activation energy threshold for compounds to react when they otherwise would not have been able to under cooler conditions.
  • thermally catalyzed interactions cause the creation of compounds which did not originate inside the reagent (i.e., the plant matter, such as a coffee bean or tea leaf) and may significantly alter the profile and chemistry of the resultant extraction.
  • hot brew systems lead to beverages that are impure in terms of chemical equivalence between the compounds originally present in the reagent and those which are now in the solvent.
  • the resulting extractions are more acidic, bitter and/or sour, as some acids, bitters and/or sours are products of the unwanted, thermally catalyzed reactions described above. Additionally, other unwanted compounds may also be produced.
  • oxidation will decrease the concentration of desired compounds (antioxidants, etc.), decrease the purity of the resultant extraction in terms of chemical equivalence between the compounds available in the reagent and those which are now in the solvent, and cause more bitterants, acids, sours and other unwanted compounds to be created from reaction chemistry with oxygen.
  • a high temperature solvent can cause relevant compounds of interest to be degraded, decomposed, denatured, vaporized, or otherwise lost.
  • Cold brew chemistry attempts to alleviate some of the above issues related to hot brewing by replacing the thermally catalyzed solvent with time and a colder solvent system (typically water at approximately l°C to 30°C). Using solvents at lower temperatures decreases the solubility of unwanted compounds, as described above, and may also decrease (and potentially eliminate) the likelihood of unwanted reactions to occur which would decrease the purity of the resulting extract.
  • a colder solvent system typically water at approximately l°C to 30°C.
  • current cold brew systems suffer a number of drawbacks. For instance, low temperature extraction results in significantly lower yield, causing the need for more reagent (2-5x more reagent) to provide an equivalent concentration of the relevant compounds in the solvent.
  • Low temperature extraction also requires extraordinarily long brew rimes (8 to 48 hours instead of a few minutes) to enable more of the solvent to infuse and dissolve all of the relevant compounds in the solvent.
  • the need for more reagent causes not only more waste, there are non-extracted compounds of interest remaining in the reagent that are unused and discarded. This increases the cost of the beverage significantly.
  • the extraordinarily long brew time also causes waste in regard to the utilization of space (cold brew needs to steep for a long time, rendering the area in which it is steeping to be otherwise unproductive), while also giving more time for the oxygenation of the solvent.
  • oxygen has ample time to dissolve into the system (similarly to how the compounds of interest are given ample time to dissolve into the solvent), creating a beverage that is even more oxygenated than its hot brewed counterpart. This is particularly harmful to some compounds of interest that degrade in the presence of oxygen (even without thermal catalysis) such as antioxidants.
  • an analyte extraction apparatus in accordance with the present invention generally comprises an extraction vessel and a sonication vessel.
  • the extraction vessel is configured to receive an extraction solvent and a solute mass.
  • the sonication vessel is adapted to receive the extraction vessel therein.
  • a gap is formed between an outer surface of the extraction vessel and an inner surface of the sonication vessel.
  • the gap is configured to receive a bath fluid therein and the sonication vessel includes at least one ultrasonic transducer configured to deliver acoustic energy to the bath fluid and to the extraction solvent.
  • a mixer having a stir end is received within the extraction vessel and configured to stir the extraction solvent and solute mass during delivery of the acoustic energy.
  • a top panel may be configured to cover the extraction vessel and the sonication vessel. The top panel may form a seal at a top edge of the extraction vessel. The panel may aid in the prevention of unwanted materials entering the extraction vessel, such as but not limited to oxygen, debris, and bath fluid.
  • the bath fluid is temperature- regulated to maintain the extraction solvent at a temperature between about 0°C and about 20°C and the bath fluid may comprise one or more of water, surfactants, an oil, an alcohol, a glycol, a ketone, an ester and an ether.
  • the extraction solvent may be water at a temperature between about 0°C and about 20°C, and the solute mass may comprise one or more of whole coffee beans, partial coffee beans, ground coffee beans, tea leaves, hemp, marijuana, cannabis, and generally barks, roots, flowers, herbal matter, vegetables, and fruits as well as other biological or organic matter including but not limited to fungi, algae, protozoa, bacteria, and meats.
  • a method for analyte extraction an extraction may comprise: a) providing an analyte extraction apparatus including a extraction vessel configured to receive an extraction solvent and a solute mass; and a sonication vessel adapted to receive the extraction vessel therein, wherein a gap is formed between an outer surface of the extraction vessel and an inner surface of the sonication vessel, wherein the gap is configured to receive a bath fluid therein, and wherein the sonication vessel includes at least one ultrasonic transducer configured to deliver acoustic energy to the bath fluid and the extraction solvent; b) allowing the extraction solvent and the solute mass to be received within the extraction vessel; c) allowing the bath fluid to be received within at least a portion of the gap; and d) allowing the ultrasonic transducer to deliver acoustic energy to the bath fluid and the extraction solvent whereby compounds within the solute mass are extracted within the extraction solvent so as to form the extraction.
  • the analyte extraction apparatus may include a mixer having a stir end received within the extraction vessel and the method may further comprise e) allowing the mixer to stir the extraction solvent and solute mass during delivery of the acoustic energy.
  • a top panel may be configured to cover the extraction vessel and the sonication vessel. The top panel may form a seal at a top edge of the extraction vessel.
  • the bath fluid may be temperature-regulated to maintain the extraction solvent at a temperature between about 0°C and about 20°C and the bath fluid may comprise one or more of water, surfactants, an oil, an alcohol, a glycol, a ketone, an ester and an ether.
  • the extraction solvent may be water at a temperature between about 0°C and about 20°C, and the solute mass may comprise one or more of whole coffee beans, partial coffee beans, ground coffee beans, tea leaves, hemp, marijuana, cannabis, and generally barks, roots, flowers, herbal matter, vegetables, and fruits as well as other biological or organic matter including but not limited to fungi, algae, protozoa, bacteria, and meats.
  • FIG. 1A is a schematic view of an analyte extraction apparatus in accordance with the present invention.
  • FIG. 1B is an additional schematic view of the analyte extraction apparatus in accordance with the present invention
  • FIG. 1C is an additional schematic view of an analyte extraction apparatus in accordance with the present invention
  • FIG. 2 is a flow chart of an exemplary method of extracting analyte in accordance with the present invention.
  • analyte extraction apparatus 10 generally comprises an extraction vessel 12 received within a sonication vessel 14. As illustrated in FIG. 1A, a gap 16 is located between outer wall 18 of extraction vessel 12 and inner wall 20 of sonication vessel 14. Gap 16 receives a bath fluid 22 therein, as will be discussed in greater detail below. Extraction vessel 12 receives an extraction solvent 24 and solute mass 26 therein.
  • extraction solvent 24 may contain, but is not limited to, any potable fluid such as water, but may also contain solids and gases (such as ice or hydrogen gas).
  • Solute mass may be any suitable material, such as and without limitation thereto, one or more of whole coffee beans, partial coffee beans, ground coffee beans, tea leaves, hemp, marijuana, cannabis, and generally barks, roots, flowers, herbal matter, vegetables, and fruits as well as other biological or organic matter including but not limited to fungi, algae, protozoa, bacteria, and meats.
  • solvent 24 and solute mass 26 are kept cold, such as between about 0°C and about 20°C).
  • the extraction vessel is comprised of glass.
  • sonication vessel 14 is equipped with one or more ultrasonic transducers 28.
  • Ultrasonic transducers 28 are positioned and configured to deliver acoustic energy to bath fluid 22 which is then transferred to extraction solvent 24.
  • bath fluid 22 may comprise one or more of water, surfactants, an oil, an alcohol, a glycol, a ketone, an ester and an ether.
  • extraction vessel 12 is constructed of material which conducts sonic vibrations.
  • Passive (indirect) cavitation is created by delivering acoustic energy not directly to the solvent, but through a bath/medium which indirectly transfers the energy to the solvent system.
  • analyte extraction apparatus 10 can increase the pressure locally within extraction vessel 12, thus increasing the solubility of the relevant compounds, without localized and/or intense heating of extraction solvent 24 or solute mass 26.
  • the passive cavitation increases the frequency of interaction between the solvent and solute, similar to the increase in solubility of the higher temperature solvent, but without affecting the activation energy barrier so that unwanted reaction chemistry does not occur because there is insufficient thermal energy in the system. Decomposition of compounds is also alleviated in contrast to hot solvent extraction (hot brewing), due to the maintenance of a lower temperature system.
  • analyte extraction apparatus 10 is thermally regulated. If analyte extraction apparatus 10 were to be left thermally unregulated, any sort of soni cation would increase the temperature of the system, thereby losing the chemical benefits of a cold extraction. In one example, the increase in temperature is a natural result of the sonication. In heretofore sonication systems, ultrasonic energy has been directly applied to the solvent/solute mass, thereby causing localized areas of intense heating and resultant corruption of the liquid, as described above. Thus, the present invention implements passive cavitation with strict temperature regulation.
  • Ultrasonic energy produced by transducer 28 is passively transferred to extraction vessel 12 via bath fluid 22 filling gap 16 between extraction vessel 12 and sonication vessel 14.
  • bath fluid 22 filling gap 16 between extraction vessel 12 and sonication vessel 14.
  • analyte extraction apparatus 10 may extract compounds that would normally be soluble only at higher temperatures (these high temperatures, however, would also degrade some or all of those compounds).
  • a beverage produced in accordance with the present invention will have a distinctly unique profile and characteristics compared to hot brewing and traditional cold brewing techniques.
  • analyte extraction apparatus 10 may extract analyte from coffee beans/grounds to create emulsions of typically insoluble compounds in an aqueous extraction.
  • analyte extraction apparatus 10 may complete an extraction cycle 5-50 times faster than traditional cold brew techniques.
  • a complete extraction cycle for producing coffee beverage may take less than 2 hours.
  • analyte extraction apparatus 10 may additionally include a mixer 30. Without consistent stirring via mixer 30, only that portion 32 of solute mass 26 which is in direct contact with extraction solvent 24 would be affected by the sonic energy.
  • mixer 30 may include a motor unit 34 located externally sonication vessel 14.
  • a shaft 36 may connect motor unit 34 to stir end 38 whereby actuation of the motor causes stir end 38 to stir extraction solvent 26 and disperse solute mass 26 within the solvent.
  • mixer 30 is configured to create a homogenous distribution of the solute mass within the sonically charged extraction solvent.
  • the solute mass 26 is mixed in with the solvent 24 with an increased surface area of particles of the solute mass 26 in contact with the solvent when sonicated during the extraction process.
  • the rate of infusion of desired compounds within solute mass 26 into extraction solvent 24 may increase.
  • analyte extraction apparatus 10 may further include a top panel 40.
  • Top panel 40 may he proportioned to cover extraction vessel 12 and sonication vessel 14, or may he proportioned only to cover extraction vessel 12.
  • Top panel 40 may further form a seal against top edge 42 of extraction vessel 12.
  • Top panel 40 may provide a number of functions. For instance, top panel 40 may prevent unwanted substances from entering into extraction vessel 12 during an extraction cycle. Top panel 40 may also prevent or minimize any evaporation of extraction solvent 24 during an extraction cycle. Additionally, top panel 40 may also limit introduction of atmospheric oxygen within headspace 44 during extraction, and thus minimize the potential for unwanted oxidation of the compounds extracted during the extraction process.
  • a method for optimized select analyte extraction is generally indicated by reference numeral 200.
  • an analyte extraction apparatus including a extraction vessel and a sonication vessel is provided.
  • a gap is formed between an outer surface of the extraction vessel and an inner surface of the sonication vessel.
  • an extraction solvent and the solute mass are allowed to be received within the extraction vessel.
  • a bath fluid is allowed to be received within at least a portion of the gap.
  • An ultrasonic transducer included within the sonication vessel is allowed to deliver acoustic energy to the bath fluid at step 208, wherein the acoustic energy is then transferred to the extraction solvent.
  • analyte extraction apparatus 10 may further comprise a mixer having a stir end received within the extraction vessel.
  • the mixer may be allowed to stir the extraction solvent and solute mass before, and/or after, and/or during delivery of the acoustic energy.
  • method 100 directs acoustic energy to a bath fluid rather than directly to the extraction solvent, the passive sonication and cavitation allows the energy to disperse more evenly within the extraction vessel. As a result, compounds of interest are extracted from the solute mass homogeneously and grinding of the mass is prevented.
  • the external bath fluid transfers the sonic energy from the transducer to the bath which spreads the energy from localized points of sonication and distributes the energy through the extraction vessel, which in turn enables homogeneous distribution of sonic energy to the solvent/solute mixture.
  • the extraction solvent is thermally regulated to have a temperature between about 0°C and about 20°C, and more preferably between about 0°C and about l0°C, and still more particularly between about 0°C and about 5°C.
  • the temperature is regulated to about 0°C for coffee extraction.
  • the temperature is regulated for biologically active proteins.
  • thermal regulation of the extraction solvent (and solute mass) is a critical factor in analyte extraction systems, particularly the use of near freezing water as the medium for cold extraction.
  • hom sonicators create high energy in a small space and direct sonication of the extraction solvent may thermally degrade the materials close to the tip.
  • systems which use hom sonicators typically sonicate on the order of 30-60 seconds.
  • sonication may last from 5 to 120 minutes due to the need for passive sonication which preserves thermal control of the solute/solvent system so as not to cause overheating.
  • the extraction solvent temperature gets too high, it can impart a burnt, oxidized, and vamish-like taste to the resultant extraction.
  • bath fluid 22 may further include a salt dissolved therein.
  • the salt may not only help keep bath fluid 22 cool, but the salt may also help absorb some of the excess energy that would otherwise go into heating the bath fluid.
  • photonics may also be integrated within the system to increase the speed of the extraction. That is, light having a proper wavelength may create excited states in materials that change the materials’ polarity and electrochemical configuration. Photonically stimulating the solvent and/or solute may accelerate the extraction and further decrease the extraction time.
  • select wavelengths in the system ranging from microwaves to ultraviolet (“UV”), with different wavelengths in between such as infrared, visible spectrum, and radar, may be used to stimulate the solute, solvent, or cosolvent and cosolvents, thereby enhancing the solubility and capture of selected analyte in the solvent.
  • the wavelengths can range from 10 3 meters to 10 10 meters.
  • the photonic stimulation may further be used to create new desired compounds or destroy undesired compounds from dissolving into the solvent.
  • one or more sensors may be added to apparatus 10 which may be configured to detect, record, and/or regulate temperature automatically.
  • one or more sensor 52 can be configured to sense temperature for temperature regulation, sampling by a spectrometer 54, pressure, time lapse, photodetector for detecting and tuning input light.
  • a spectrophotometer may also be used to determine when the solution (beverage) indicates that the compounds of interest have been sufficiently extracted/infused within the solvent, thereby optimizing time required to extract.
  • a pressure control system is configured to regulate pressure in the extraction vessel 12.
  • the pressure control system can deliberately pressurize or depressurize the solution in the extraction vessel 12 to enhance or increase the solubility of the desired analyte and minimize the solubility of undesired compounds.
  • the pressure control system includes one or more sensors 52 located beneath or inside top edge 42 configured to collect pressure information.
  • the one or more sensors of the pressure control system can be part of the top penal measuring pressure of the headspace.
  • the photonic and pressure systems can be used separately or in conjunction with the temperature controlled passive sonication system.
  • the one or more sensors 52 including one or more spectrometers, one or more spectrophotometers, or both, can communicate with external devices and to a data log.
  • the sensors 52 can be located within the top edge 42, above top edge 42, or suspended beneath top edge 42 and periodically or continuously sample solvent for analysis.
  • a sample solvent can be received by a tube or port and piped up through the tube or port to the spectrophotometer for sampling.
  • the sample would be diluted to give readings in the proper detection limit or zone.
  • the input variables such as light intensity & color of the solute mass 26 or solution, temperature, stir rate, photonic energy including frequency and intensity, can also be manipulated and regulated remotely on an electronic device or similar device.
  • the device can communicate, periodically or continuously, with, or operated by, an external server, computer, or controller.

Abstract

La présente invention concerne un appareil d'extraction d'analyte qui comprend un récipient d'extraction et un récipient de sonication. Le récipient d'extraction reçoit un solvant d'extraction et une masse de soluté, et le récipient de sonication reçoit le récipient d'extraction à l'intérieur de celui-ci. Un espacement est formé entre une surface externe du récipient d'extraction et une surface interne du récipient de sonication. L'espacement reçoit un fluide de bain et le récipient de sonication comprend au moins un transducteur ultrasonore pour délivrer une énergie acoustique au fluide de bain et au solvant d'extraction. Le fluide de bain est régulé en température pour maintenir le solvant d'extraction à une température définie. L'appareil d'extraction d'analyte peut comprendre en outre un mélangeur pour agiter le solvant d'extraction et la masse de soluté pendant la distribution de l'énergie acoustique.
PCT/US2019/057151 2018-10-23 2019-10-21 Dispositif et procédé d'extraction d'analyte de sélection optimisé WO2020086431A1 (fr)

Applications Claiming Priority (2)

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US201862749166P 2018-10-23 2018-10-23
US62/749,166 2018-10-23

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PCT/US2019/057153 WO2020086432A1 (fr) 2018-10-23 2019-10-21 Dispositif et procédé d'extraction d'analyte de sélection optimisée

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5484573A (en) * 1992-08-28 1996-01-16 Hoechst Aktiengesellschaft Reactor for carrying out chemical reactions
WO1997022398A1 (fr) * 1995-12-18 1997-06-26 Ixtlan Ag Procede et appareil pour filtrer des substances liquides ou pateuses et/ou pour separer des composants inclus dans ces substances
US20030113797A1 (en) * 2001-06-27 2003-06-19 Unigen Pharmaceuticals, Inc. Method for generating, screening and dereplicating natural product libraries for the discovery of therapeutic agents
WO2005063962A1 (fr) * 2003-12-24 2005-07-14 Drug Risk Solutions, Inc. Systeme pour la comminution, l'extraction et la detection d'analytes dans des echantillons biologiques solides
KR20170049124A (ko) * 2015-10-28 2017-05-10 전주대학교 산학협력단 프로폴리스 유효성분 추출장치 및 추출방법
US9863090B2 (en) * 2013-02-27 2018-01-09 Bio-Sep Limited Process operations for biomass fractionation

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5484573A (en) * 1992-08-28 1996-01-16 Hoechst Aktiengesellschaft Reactor for carrying out chemical reactions
WO1997022398A1 (fr) * 1995-12-18 1997-06-26 Ixtlan Ag Procede et appareil pour filtrer des substances liquides ou pateuses et/ou pour separer des composants inclus dans ces substances
US20030113797A1 (en) * 2001-06-27 2003-06-19 Unigen Pharmaceuticals, Inc. Method for generating, screening and dereplicating natural product libraries for the discovery of therapeutic agents
WO2005063962A1 (fr) * 2003-12-24 2005-07-14 Drug Risk Solutions, Inc. Systeme pour la comminution, l'extraction et la detection d'analytes dans des echantillons biologiques solides
US9863090B2 (en) * 2013-02-27 2018-01-09 Bio-Sep Limited Process operations for biomass fractionation
KR20170049124A (ko) * 2015-10-28 2017-05-10 전주대학교 산학협력단 프로폴리스 유효성분 추출장치 및 추출방법

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