WO2020086432A1 - Device and method for optimized select analyte extraction - Google Patents

Device and method for optimized select analyte extraction Download PDF

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Publication number
WO2020086432A1
WO2020086432A1 PCT/US2019/057153 US2019057153W WO2020086432A1 WO 2020086432 A1 WO2020086432 A1 WO 2020086432A1 US 2019057153 W US2019057153 W US 2019057153W WO 2020086432 A1 WO2020086432 A1 WO 2020086432A1
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Prior art keywords
extraction
vessel
solvent
analyte
bath fluid
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PCT/US2019/057153
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French (fr)
Inventor
James SINKA
Andrew FLEISCHER
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Moonshot Brewing Holdings, Inc.
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Application filed by Moonshot Brewing Holdings, Inc. filed Critical Moonshot Brewing Holdings, Inc.
Publication of WO2020086432A1 publication Critical patent/WO2020086432A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/028Flow sheets
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F5/00Coffee; Coffee substitutes; Preparations thereof
    • A23F5/24Extraction of coffee; Coffee extracts; Making instant coffee
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0211Solvent extraction of solids in combination with an electric or magnetic field
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0215Solid material in other stationary receptacles
    • B01D11/0253Fluidised bed of solid materials
    • B01D11/0257Fluidised bed of solid materials using mixing mechanisms, e.g. stirrers, jets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0261Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • B01D11/0265Applying ultrasound

Definitions

  • the present invention relates to brewing techniques and devices; and more particul arly to analyte extraction techniques and devices; and even more parti cularly to analyte extraction techniques and devices for extracting bioavailable compounds from plants.
  • 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.
  • high temperature solvent extraction leads to an increased likelihood for oxidation. Similar to the chemical principles described above, the higher temperature solvent will actively dissolve more oxygen from the ambient environment, providing an abundance of oxygen for oxygen related chemistries to occur. This is particularly harmful to the extraction because of the high concentration of antioxidants and other key compounds that are oxygen sensitive that are originally present in the reagents. Furthermore, the higher frequency of collisions, due to temperature of the hot solvent, significantly increases the rate and likelihood of the oxidation of these compounds. Finally, the thermally catalyzed system (hot brewing) will also enable more oxygen chemistry to occur when compared to lower temperature brewing systems due to the required activation energy gained from a high temperature environment.
  • 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 loC to 30oC). 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.
  • 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 times (8 to 48 hours instead of a fe minutes) to enable more of the solvent to infuse and di ssolve 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 QoC and about 2(3oC 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 OoC and about 20oC, 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 GoC and about 20oC 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 QoC and about 20oC, 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. 1 A is a schematic view of an analyte extraction apparatus in accordance with the present invention.
  • FIG. IB 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 wit 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 a extraction vessel 12 received within a sonication vessel 14. As i llustrated in FIG. I A, 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, or alcohol or glycerin, 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 harks, 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 OoC and about 20oC).
  • the extraction vessel 12 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.
  • the solvent 24 in extraction vessel 12 can include glycerin, alcohol, or a combination thereof.
  • the solvent 24 and bath fluid 22 are comprised of different material.
  • the extraction vessel 12 is compri sed of a metallic material.
  • 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 sonication would increase the temperature of the system, thereby losing the chemical benefits of a cold extraction. 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. Thus, any thermal energy experienced by extraction solvent 24 in extraction vessel 12 is minimized and distributed (therefore not localized as it would be found in traditional ultrasonication systems).
  • the extraction solvent 24/solute mass 26 mixture may stay substantially free from thermal degradation and/or chemical reaction products. Due to the higher pressure and frequency of interaction between extraction solvent 24 and solute mass 26, 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). As a result, and in accordance with one aspect of the present invention, 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.
  • solutes that are readily soluble at the extraction temperatures used within the present invention (OoC to about 20oC) are quickly extracted due to the high frequency of collisions between the solute mass 26 and extraction solvent 24.
  • 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. For example, as illustrated in FIG.
  • analyte ex traction apparatus 10 may further include a top panel 40.
  • Top panel 40 may be proportioned to cover extraction vessel 12 and sonication vessel 14, or may be 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 extracti on, and thus minimize the potential for unwanted oxi dation 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 allow-ed 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 di stribution of sonic energy to the solvent/solute mixture.
  • the horn method creates highly localized, high-energy hot zones that make it an ineffective technique for creating a true extraction because of the intense localized heat that ruins the chemical benefits of analyte extraction described above. That is, by the time the surrounding environment can equilibrate the temperature introduced by the ultrasonic horn, the local solute and solvent mix has been thermally catalyzed causing localized hot brew chemistry, with all the negative effects of hot brewing as described above.
  • the extraction solvent is thermally regulated to have a temperature between about OoC and about 20oC, and more preferably between about OoC and about lOoC, and still more particularly between about OoC and about 5oC.
  • temperature regulation can facilitate optimizing select analyte extraction of cannabinoids in cannabis while reducing the extraction of unwanted compounds such as chlorophyll.
  • 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 varnish-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 103 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 soni cation 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

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
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Abstract

An analyte extraction apparatus includes an extraction vessel and a sonication vessel. The extraction vessel receives an extraction solvent and a solute mass, and the sonication vessel receives 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 receives a bath fluid therein and the sonication vessel includes at least one ultrasonic transducer to deliver acoustic energy to the bath fluid and extraction solvent. The bath fluid is temperature-regulated to maintain the extraction solvent at set temperature. The analyte extraction apparatus may also include a mixer to stir the extraction solvent and solute mass during delivery of the acoustic energy.

Description

DEVICE AND METHOD FOR OPTIMIZED SELECT ANALYTE EXTRACTION
FIELD OF THE IN VENTION
[0001] The present invention relates to brewing techniques and devices; and more particul arly to analyte extraction techniques and devices; and even more parti cularly to analyte extraction techniques and devices for extracting bioavailable compounds from plants.
BACKGROUND OF THE INVENTION
[0002] When water is added to plant material, it acts as the solvent that dissolves the soluble compounds in the plant material. Temperature is directly related to solubility, such that the higher the temperature of the solvent (typically water), the higher the solubility of the compounds. In traditional hot extraction systems (i.e., hot water extractions usually using water at approximately 70°C to 100°C) the high solubility of the hot water causes ail relevant compounds to be extracted in a relatively short time 3-10 minutes. The upside of this is fast throughput and high yield as less reagent is required to reach a desired concentration of the compounds in the solvent (water) because a high percentage of the relevant compounds are naturally more soluble in the hot water. One of the downsides of hot extraction, however, is that the solubility of the compounds is uncontrolled and therefore all compounds that can be thermally extracted are. In the case of cannabis, these compounds may include those which imbue an unpleasant experience due to, but not limited to, bitterants
[0003] 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. These thermally catalyzed interactions cause the creation of compounds which did not originate inside the reagent (i.e., the plant matter, such as cannabis and hemp) and may significantly alter the profile and chemistry of the resultant extraction. As a result, hot extraction systems lead to products 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. For example, in cannabinoid extraction, such as THC extraction of cannabis, increasing the rate at which THC is extracted can also increase the rate of undesired chlorophyll.
10004] Moreover, high temperature solvent extraction leads to an increased likelihood for oxidation. Similar to the chemical principles described above, the higher temperature solvent will actively dissolve more oxygen from the ambient environment, providing an abundance of oxygen for oxygen related chemistries to occur. This is particularly harmful to the extraction because of the high concentration of antioxidants and other key compounds that are oxygen sensitive that are originally present in the reagents. Furthermore, the higher frequency of collisions, due to temperature of the hot solvent, significantly increases the rate and likelihood of the oxidation of these compounds. Finally, the thermally catalyzed system (hot brewing) will also enable more oxygen chemistry to occur when compared to lower temperature brewing systems due to the required activation energy gained from a high temperature environment. As a result, 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. Additionally, a high temperature solvent can cause relevant compounds of interest to be degraded, decomposed, denatured, vaporized, or otherwise lost.
[0005] Another important consideration is the particle size of the material being brewed
(i.e , marijuana leaves.). In general, with a smaller particle size, there is a larger surface area of interaction, therefore increasing extraction kinetics. A smaller size, assuming all other variables constant, results in a more complete extraction. There are, however, downsides to using smaller sized particles - for example, selective extraction is far more difficult. Selecting a particle size that delivers controllable extraction kinetics and the most desired flavor profile is therefore desired. Optimal size varies from origin, preparation style, and other factors, but must remain consistent throughout. Particle size can change during the extraction process depending on the extraction method, and as a result, maintaining consistent particle size throughout the extraction process is of paramount importance. Also, complete or equivalent extractions can be produced with a larger particle size when compensating with added time. Once a recipe has been established, changing the particle size may alter the processing of the beverage, therefore changing and potentially ruining the recipe for that beverage.
[0006] 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 loC to 30oC). 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. However, 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 times (8 to 48 hours instead of a fe minutes) to enable more of the solvent to infuse and di ssolve 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. During the long brewing time, 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
[0007] As a result of the above, traditional cold brew is far more costly than its hot brewed counterpart - with respect to time, money, and space, may be more oxidized than its hot brewed counterpart, thereby decreasing some of its chemical value, i.e., fewer free/non- oxidized antioxidants; contains fewer compounds of i nterest because they are not soluble at the lower temperature; and contains fewer umvanted compounds such as bitterants, acids, sour notes, and burnt tastes. [0008] Thus, what is needed in the art is an analyte extraction system and method that affords faster brewing than traditional cold brewing but retains, and improves upon, the benefits of traditional cold brewing over hot brewing technologies. The present invention satisfies these, and other, needs.
SUMMARY OF THE INVENTION
[0009] Briefly described, 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.
[0010] In a further aspect of the present invention, 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. Additionally, or alternatively, 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.
[0011] In another aspect of the present invention, the bath fluid is temperature- regulated to maintain the extraction solvent at a temperature between about QoC and about 2(3oC 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 OoC and about 20oC, 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.
[0012] In still another aspect of the present invention, 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.
[0013] In a further aspect of the present invention, 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. Additionally, or alternatively, 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 GoC and about 20oC 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 QoC and about 20oC, 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.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 A is a schematic view of an analyte extraction apparatus in accordance with the present invention;
[0015] FIG. IB is an additional schematic view of the analyte extraction apparatus in accordance with the present invention;
[0016] FIG. 1C is an additional schematic view of an analyte extraction apparatus in accordance wit the present invention; [0017] FIG. 2 is a flow chart of an exemplary method of extracting analyte in accordance with the present invention.
DETAILED DESCRIPTION OF A PREFERRED EMBODIMENT
[0018] Referring to the drawings in detail, and specifically to FIG 1A-C, analyte extraction apparatus 10 generally comprises a extraction vessel 12 received within a sonication vessel 14. As i llustrated in FIG. I A, 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. By way of example and without limitation thereto, extraction solvent 24 may contain, but is not limited to, any potable fluid such as water, or alcohol or glycerin, 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 harks, 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. To minimize the solubility of unwanted compounds and/or their creation, solvent 24 and solute mass 26 are kept cold, such as between about OoC and about 20oC). In one aspect, the extraction vessel 12 is comprised of glass
!;ooi9! To facilitate extraction of desired compounds from solute mass 26 so as to infuse extraction solvent 24 and produce the resultant extraction, 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 By way of example and without limitation thereon, bath fluid 22 may comprise one or more of water, surfactants, an oil, an alcohol, a glycol, a ketone, an ester and an ether.
[0020] In one example, to extract cannabinoids from cannabis, the solvent 24 in extraction vessel 12 can include glycerin, alcohol, or a combination thereof. In another example, the solvent 24 and bath fluid 22 are comprised of different material. In another example, the extraction vessel 12 is compri sed of a metallic material.
[0021] To enable transfer of the acousti c energy, 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. As a result, 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.
[0022] In accordance with an aspect of the present invention, analyte extraction apparatus 10 is thermally regulated. If analyte extraction apparatus 10 were to be left thermally unregulated, any sort of sonication would increase the temperature of the system, thereby losing the chemical benefits of a cold extraction. 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. Thus, any thermal energy experienced by extraction solvent 24 in extraction vessel 12 is minimized and distributed (therefore not localized as it would be found in traditional ultrasonication systems).
[0023] Due to the thermal regulation and buffering afforded by bath fluid 22, the extraction solvent 24/solute mass 26 mixture may stay substantially free from thermal degradation and/or chemical reaction products. Due to the higher pressure and frequency of interaction between extraction solvent 24 and solute mass 26, 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). As a result, and in accordance with one aspect of the present invention, 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. By way of example and without limitation thereto, analyte extraction apparatus 10 may extract analyte from coffee beans/grounds to create emulsions of typically insoluble compounds in an aqueous extraction. 10024] Furthermore, the solutes that are readily soluble at the extraction temperatures used within the present invention (OoC to about 20oC) are quickly extracted due to the high frequency of collisions between the solute mass 26 and extraction solvent 24. As a result, analyte extraction apparatus 10 may complete an extraction cycle 5-50 times faster than traditional cold brew techniques. In accordance with an aspect of the present invention, a complete extraction cycle for producing coffee beverage may take less than 2 hours.
10025] In a further aspect of the present invention, to further increase the distribution and surface area of the particles comprising solute mass 26 within extraction solvent 24, 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. By way of example, 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. In accordance with an aspect of the present invention, mixer 30 is configured to create a homogenous distribution of the solute mass within the sonically charged extraction solvent. For example, as illustrated in FIG. IB, when mixer 30 is stirring the solution, 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. As a result of stirring, the rate of infusion of desired compounds within solute mass 26 into extraction solvent 24 may increase.
[0026] In another aspect of the present invention, analyte ex traction apparatus 10 may further include a top panel 40. Top panel 40 may be proportioned to cover extraction vessel 12 and sonication vessel 14, or may be 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 extracti on, and thus minimize the potential for unwanted oxi dation of the compounds extracted during the extraction process.
[0027] Turning now to FIG. 2, a method for optimized select analyte extraction is generally indicated by reference numeral 200. At step 202 of method 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. At step 204, an extraction solvent and the solute mass are allowed to be received within the extraction vessel. At step 206, 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. The transferred energy may then extract compounds within the solute mass to infuse the extraction solvent and form the extract. In a further aspect of the present invention, analyte extraction apparatus 10 may further comprise a mixer having a stir end received within the extraction vessel. At step 210, the mixer may be allow-ed to stir the extraction solvent and solute mass before, and/or after, and/or during delivery- of the acoustic energy.
[0028] Because 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 di stribution of sonic energy to the solvent/solute mixture.
[0029] In contrast, current systems use an ultrasonic horn to deliver sonication directly to the water and solute mass (i.e., coffee bean) which further grinds the material and increases the surface area of the organic matter, thereby changing the extraction and its original extraction kinetics. In one aspect of the present invention, the particle size of the plant matter is specifically predetermined to control the solubility characteristics and quality of the resultant extraction, such as a beverage. Thus, changing the particle size through the horn sonication is detrimental as it affects the required control over the extraction process. Furthermore, deliver}- of sonication through an ultrasonic horn/tip delivers the energy non-homogeneously, causing inconsistencies in extraction and temperature distribution. The horn method creates highly localized, high-energy hot zones that make it an ineffective technique for creating a true extraction because of the intense localized heat that ruins the chemical benefits of analyte extraction described above. That is, by the time the surrounding environment can equilibrate the temperature introduced by the ultrasonic horn, the local solute and solvent mix has been thermally catalyzed causing localized hot brew chemistry, with all the negative effects of hot brewing as described above.
[0030] In accordance with an aspect of the present invention, the extraction solvent is thermally regulated to have a temperature between about OoC and about 20oC, and more preferably between about OoC and about lOoC, and still more particularly between about OoC and about 5oC. For example, temperature regulation can facilitate optimizing select analyte extraction of cannabinoids in cannabis while reducing the extraction of unwanted compounds such as chlorophyll. In one aspect of the present invention, 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. As discussed above, if the extraction solvent temperature gets too high, it can impart a burnt, oxidized, and varnish-like taste to the resultant extraction.
[0031] In a further aspect of the present invention, 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. Still further, 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. In one aspect, 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 103 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.
[0032] In a further aspect, one or more sensors may be added to apparatus 10 which may be configured to detect, record, and/or regulate temperature automatically. For example, 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. Additionally, or alternatively, 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. 10033] In a further aspect, as illustrated in FIG. 1C, 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. In one example, the pressure control system includes one or more sensors 52 located beneath or inside top edge 42 configured to collect pressure information. In one example, the one or more sensors of the pressure control system can be part of the top penal measuring pressure of the headspace.
[0034] In a further aspect, the photonic and pressure systems can be used separately or in conjunction with the temperature controlled passive soni cation system
[0035] In a further aspect, 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. In one example, a sample solvent can be received by a tube or port and piped up through the tube or port to the spectrophotometer for sampling. In one example, 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
[0036] Although the present invention has been described in considerable detail with reference to certain aspects thereof, other versions are possible. Therefore, the spirit and scope of the appended claims should not be limited to the description of the aspects contained herein.
[0037] All features disclosed in the specification, including the claims, abstract, and drawings, and all the steps in any method or process disclosed, may be combined in any combination, except combinations where at least some of such features and/or steps are mutually exclusive. Each feature disclosed in the specification, including the claims, abstract, and drawings, can be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise. Thus, unless expressly stated otherwise, each feature disclosed is one example only of a generic series of equivalent or similar features.

Claims

WHAT IS CLAIMED IS:
1. An analyte extraction apparatus comprising: an 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.
2 The analyte extraction apparatus of claim 1, further comprising: a mixer having a stir end received within the extraction vessel and configured to stir the extraction solvent and solute mass during deliver}' of the acoustic energy.
3. The analyte extraction apparatus of claim 1, further comprising: a top panel configured to cover the extraction vessel and the sonication vessel.
4. The analyte extraction apparatus of claim 3, wherein the top panel forms a seal at a top edge of the extraction vessel.
5. The analyte extraction apparatus of claim 1, wherein the bath fluid is temperature- regulated to maintain the extraction solvent at a temperature between about 0°C and about 50°C.
6. The analyte extraction apparatus of claim 1, wherein the bath fluid comprises one or more of water, surfactants, an oil, an alcohol, a glycol, a ketone, an ester and an ether.
7. The analyte extraction apparatus of claim 1, wherein the extraction solvent comprises one or more of water, glycerin, and alcohol.
8. The analyte extraction apparatus of claim 1, wherein the solute mass comprises 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.
9. A method for analyte extraction, the method comprising: providing an extraction apparatus including an 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;
allowing the extraction solvent and the solute mass to be received within the extraction vessel;
allowing the bath fluid to be received within at least a portion of the gap; and 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.
10 The method of claim 9, wherein the extraction apparatus further comprises a mixer having a stir end received within the extraction vessel and wherein the method further comprises:
allowing the mixer to stir the extraction solvent and solute mass during deliver} of the acoustic energy.
allowing the mixer to homogenize the solvent/solute mixture allowing the mixer to evenly disperse any locally produced thermal activity.
11. The method of claim 9, wherein the extraction apparatus further comprises a top panel configured to cover the extraction vessel and the sonication vessel.
12. The method of claim 11, wherein the top panel forms a seal at a top edge of the extraction vessel.
13. The method of claim 9, wherein the bath fluid is temperature- regulated to maintain the extraction solvent at a temperature between about 0°C and about 50°C.
14. The method of claim 9, wherein the bath fluid comprises one or more of water, surfactant, an oil, an alcohol, a glycol, a ketone, an ester and an ether.
15. The method of claim 9, wherein the extraction solvent comprises one or more of water, glycerin, and alcohol.
16. The method of claim 9, wherein the solute mass comprises 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.
PCT/US2019/057153 2018-10-23 2019-10-21 Device and method for optimized select analyte extraction WO2020086432A1 (en)

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