WO2015106217A1 - Method for rapid maturation of distilled spirits using light and heat processes - Google Patents
Method for rapid maturation of distilled spirits using light and heat processes Download PDFInfo
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- WO2015106217A1 WO2015106217A1 PCT/US2015/011056 US2015011056W WO2015106217A1 WO 2015106217 A1 WO2015106217 A1 WO 2015106217A1 US 2015011056 W US2015011056 W US 2015011056W WO 2015106217 A1 WO2015106217 A1 WO 2015106217A1
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
- C12H1/16—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
- C12H1/165—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation by irradiation
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/04—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs
- C12G3/06—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs with flavouring ingredients
- C12G3/07—Flavouring with wood extracts, e.g. generated by contact with wood; Wood pretreatment therefor
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
- C12H1/16—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
- C12H1/18—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation by heating
Definitions
- esters are compounds made by chemically bonding acid molecules and alcohol molecules to form new compounds, often with pleasant aromas and tastes. This process is known as "esterification.”
- wood-aged spirits derive additional characteristics through other processes, including extraction of flavor compounds from the wood container (e.g., the ubiquitous oak barrel). These processes are not necessarily separate or distinct, and can interact with and affect each other.
- Carboxylic acid esters are responsible for the fruity aromas and tastes in distilled spirits.
- Carboxylic precursor acids are derived from the yeast and bacteria during fermentation. If organic materials are used for the container in which these reactions occur, those materials also influence the process. For example, where a charred or toasted oak barrel is used, carboxylic precursor acids are also derived from thermal decomposition of the oak polymer, hemi-cellulose, found in the inner lining of the barrel. Carboxylic precursor acids are largely responsible for "off-flavors" in distilled spirits.
- Phenolic aldehydes also play a major role producing aromas similar to vanilla, pipe tobacco, and smoke. Phenolic aldehydes are largely derived from thermally broken down oak polymers found within the inner lining of the barrel.
- Complex esters are responsible for complex honeyed aromas in distilled spirits. The complex esters are generally produced from the chemical reactions of both carboxylic and phenolic acids/aldehydes with alcohols during the time in the barrel or other container.
- Fischer esterification of fatty acids and alcohol is a well-understood and commonly practiced chemical reaction.
- a typical laboratory process involves heating a solution of fatty acids and alcohols under reflux in the presence of an acid catalyst.
- strong acids e.g., sulfuric acid
- Fischer esterification can also be completed using weak acid catalysts, but at the expense of relatively slow reaction rates. Where charred or toasted oak barrels are used during the maturation of distilled spirits, weak acids may be gradually extracted from organic material in the walls of the barrel.
- Wood extraction is the process that gives distilled spirits their color and astringent
- a process for producing a distilled spirit having characteristics associated with a mature spirit comprising: (a) contacting an unmatured distilled spirit with wood at a temperature between about 140° F and about 170° F for a period of time ranging from about 24 hours to about 336 hours to give a distilled spirit mixture; (b) contacting the distilled spirit mixture with wood and actinic light at a wavelength ranging from 400nm to lOOOnm for a cumulative exposure of at least 2,280,000 lux hours to give an actinic light-treated distilled spirit mixture; and (c) providing heat to the actinic light-treated distilled spirit mixture produced in step (b) to maintain a temperature between about 140° F and about 170° F for a period of time ranging from about 12 hours to about 336 hours to produce the mature spirit.
- the disclosure provides a process for producing a distilled spirit having characteristics of a mature spirit comprising, (a) contacting a first unmatured distilled spirit with wood at a temperature between about 140° F and about 170° F for a period of time ranging from about 24 hours to about 336 to give a first distilled spirit mixture; (b) contacting a second unmatured distilled spirit with wood and actinic light at a wavelength ranging from 400 nm to 1000 nm for a cumulative exposure of at least 2,280,000 lux hours to give a second distilled spirit mixture; and (c) mixing the first and second distilled spirit mixtures to produce the mature spirit.
- FIG. 1 shows the GCMS chromatogram from an unprocessed rum sample.
- FIG. 2 shows the GCMS chromatogram from a sample of a commercially available rum which has been aged for 32 years by conventional aging techniques.
- FIG. 3 shows the GCMS chromatogram from a rum sample that was subjected to heating in accordance with Example 3 but was not subjected to actinic light.
- FIG. 4 shows the GCMS chromatogram from a rum sample subjected to actinic light but not to heat in accordance with Example 4.
- FIG. 5 shows the GCMS chromatogram from a rum sample that is a mixture of rum subjected to heat and rum subjected to actinic light in accordance with Example 5.
- FIG. 6 shows the GCMS chromatogram from a rum sample that has been processed with both heat and light in accordance with Example 6.
- FIG. 7 depicts a wooden barrel for the heat process with a cutaway to show the barrel's internals.
- FIG. 8 depicts a sealed vessel for the heat process with a cutaway to show the vessels internals.
- the invention pertains to processes for producing a distilled spirit having characteristics associated with a mature distilled spirit.
- the distilled spirit produced in accordance with the process has many of the characteristics associated with a matured distilled spirit produced in accordance with industry standards, but is advantageously produced in a shortened timeframe while eliminating the evaporation problem and greatly reducing the "off flavors" associated with excess ethyl acetate.
- the maturation process can be shortened without reducing the quality of the spirit.
- the processes described herein produce a spirit having similar chemical markers as a 32 year-old spirit in a significantly reduced period of time.
- a spirit refers to any distilled spirit.
- the spirit is a sugar cane-based, grain-based, fruit-based, or agave-based spirit such as rum, tequila, mescal, whiskey, brandy, gin, or combinations thereof.
- a distilled spirit having the characteristics associated with a matured distilled spirit describes a spirit, which, by one or more chemical markers, has attained characteristics associated with spirits aged in accordance with industry standards. Such standards, for example, include aging a spirit in wood over a period of time greater than 1, 5, 10, 15, 20, 25 or 30 years. The characteristics associated with a matured distilled spirit may include taste, aroma, and body profiles, such as smoothness. [0024] Historically, ethyl acetate concentration was used as a marker for the progress of aging where higher amounts indicate greater maturation time. But, ethyl acetate is not itself desirable and adds a flavor and aroma comparable to paint thinners.
- samples of distilled spirits receiving high reviews comparable or in some cases better than an aged spirit, do not always have a high ethyl acetate concentration.
- highly prized spirits can be analyzed for their chemical make-up.
- chemical markers can be selected as a model for a mature spirit.
- these chemical markers provide advantages over the traditional measurement of ethyl acetate concentration to determine age.
- the chemical markers set forth herein are desirable for modeling purposes because, unlike ethyl acetate, the chemical markers contribute to the desired flavor profile.
- ethyl acetate concentrations are reduced to a concentration less than about 200,00C ⁇ g/L. In another embodiment, the ethyl acetate concentrations range between about 50,00C ⁇ g/L to about 170,00(Vg/L.
- a mature distilled spirit having the characteristics associated with a matured distilled spirit describes a spirit, which has attained a flavor and aroma profile organoleptically similar to spirits aged with wood for many years, and typically showing a chemical profile containing key chemical markers in particular proportions.
- a mature spirit can be characterized by the increasing concentrations of one or more chemical markers.
- Three markers in particular, are thought to be particularly useful for defining a mature spirit: sinapaldehyde, ethyl decanoate, and ethyl dodecanoate.
- Ethyl decanoate and ethyl dodecanoate are often found in unmature spirits at low concentrations.
- Sinapaldehyde is typically not found in an unmature spirit.
- a mature spirit is characterized by an increase of at least about 3X for ethyl dodecanoate over an unmature spirit.
- a mature spirit is characterized by an increase of at least about 3X for ethyl decanoate over an unmature spirit.
- Increased concentrations may be assessed by any method known in the art.
- a spirit that presents these three compounds in relative proportion typically has desirable flavor characteristics.
- a mature spirit may also be characterized by a sinapaldehyde peak greater than 80% and less than 200% of the peak height of ethyl decanoate and ethyl dodecanoate as measured by GCMS.
- sinapaldehyde concentration is disproportionately important in creating a spirit that meets the organoleptic properties of a mature spirit.
- a mature spirit is one that produces relative peak heights that are substantially similar to the peak heights shown in FIG. 5 for sinapaldehyde, ethyl decanoate, and ethyl dodecanoate.
- “Substantially similar,” as used herein, refers to a relative peak height differing by no more than 30%, no more than 25%, no more than 20%, no more than 15%, no more than 10%, no more than 5%, or no more than 2%.
- a mature spirit is one that produces relative peak heights that are substantially similar to the relative peak heights shown in FIG.
- a mature spirit is one that produces relative peak heights that are substantially similar to the relative peak heights shown in FIG. 5 for sinapaldehyde, ethyl decanoate, ethyl dodecanoate, acetyl, and syringaldehyde.
- a mature spirit is one that produces relative peak heights that are substantially similar to the relative peak heights shown in FIG. 6 for sinapaldehyde, ethyl decanoate, and ethyl dodecanoate.
- a mature spirit is one that produces relative peak heights that are substantially similar to the relative peak heights shown in FIG. 6 for sinapaldehyde, ethyl decanoate, ethyl dodecanoate, and acetyl.
- a mature spirit is one that produces relative peak heights that are substantially similar to the relative peak heights shown in FIG. 6 for sinapaldehyde, ethyl decanoate, ethyl dodecanoate, acetyl, and syringaldehyde.
- the unmatured distilled spirit is a spirit that has not attained the markers or characteristics associated with a matured distilled spirit.
- the "unmatured distilled spirit,” as described herein, refers to white or raw spirits, as well as partially matured spirits, provided that the unmatured distilled spirit is lacking in certain characteristics of a matured spirit.
- the unmatured distilled spirit, as described herein, has an alcohol content of at least 50% by volume. In some embodiments, the alcohol content of the unmature distilled spirit is between 50% and 80% by volume.
- distillate mixture refers to any distillate on the spectrum from matured to unmatured.
- distillate refers to the liquid composition in the vessel and may include an unmatured distilled spirit, a matured distilled spirit, or a distilled spirit mixture.
- the unmatured distilled spirit is contacted with wood in a vessel.
- the wood is provided as the vessel for holding the distillate.
- the vessel is, for example, an oak barrel.
- wood may be provided to the inside of the reaction vessel, which is optionally made of wood.
- wood chips may be added such that they are submerged or floating on top of the distillate.
- Wood may also be provided as various structural configurations within the vessel including as baffles or packing.
- wood may include wood extracts and raw acids designed to mimic the characteristics of wood.
- the wood is oak.
- One aspect of the present invention provides a process for producing a mature spirit using sequential temperature and light processing.
- the process comprises the steps of (a) contacting an unmatured distilled spirit with wood at a temperature between about 140° F and about 170° F for a period of time ranging from about 24 hours to about 336 hours to give a distilled spirit mixture; (b) contacting the distilled spirit mixture with wood and actinic light at a wavelength ranging from 400nm to lOOOnm for a cumulative exposure of at least 2,280,000 lux hours to give an actinic light-treated distilled spirit mixture; and (c) providing heat to the actinic light-treated distilled spirit mixture produced in step (b) to maintain a temperature between about 140° F and about 170° F for a period of time ranging from about 12 hours to about 336 hours to produce the mature spirit.
- the unmatured spirit is be subjected to thermal processing.
- the unmatured distilled spirit is contacted with the wood at a temperature ranging from about 140° F to about 170° F.
- the temperature ranges from about 140° F to about 150 0 F, from about 145° F to about 150° F, from about from about 150° F to about 160° F, or from about 160° F to about 170 0 F.
- the time period needed to convert the unmatured distilled spirit to a distilled spirit mixture having partial characteristics associated with a matured spirit depends on factors such as the starting composition of the unmatured distilled spirit and the temperature at which the process is conducted. In some embodiments, a temperature between about 140° F and about 170° F is provided for a period of time ranging from about 12 hours to about 336 hours.
- a temperature between about 140° F and about 170° F is provided for a period of time ranging from about 12 hours to about 24 hours, from about 24 hours to about 48 hours, from about 48 hours to about 96 hours, from about 96 hours to about 168 hours, from about 168 hours to about 226 hours, or from about 226 hours to about 336 hours.
- the heating is conducted in a sealed vessel or under reflux such that evaporation of volatile compounds is prevented.
- the pressure inside the vessel can and will vary in different embodiments of the invention. In general, the internal pressure of the vessel housing the reaction components climbs to a maximum of about 6 pounds per square inch (psi). The typical range of pressures in the vessel is between 2 psi and 6 psi, but can be altered to relieve pressure and maintain an operating pressure of less than 1 psi while still achieving the desired chemical reactions.
- the temperature is maintained between about 140° F and about 150° F for a period of time ranging from about 168 hours to about 226 hours.
- the temperature is maintained between about 150° F and about 160° F for a period of time ranging from about 24 hours to about 72 hours.
- heat is applied continuously through the given time period. But, heat may also be provided for the given time period in a manner that is not continuous, for example, at intervals so long as heat is provided totaling the stated time period.
- a first distilled spirit mixture is provided. In this embodiment of the invention, the first distilled spirit mixture produced by the heat process is further reacted as described below.
- the heat process may be conducted in an apparatus as shown in FIG. 7, which shows a cutaway view of one possible internal configuration.
- the vessel 1 may be a wooden barrel.
- FIG. 8 a cutaway is shown using dashed lines to reveal another possible internal confirmation of the vessel 1, where vessel 1 may be a stainless steel container.
- the wood 12 is provided as chips or planks submerged in or floating on top of the distillate 2.
- heat may be applied to the distillate 2 inside the vessel 1 via a heat source 4.
- the vessel is sealed under pressure.
- the vessel is heated under reflux to prevent evaporation of volatile compounds. Any method for introducing sufficient heat to the distillate including an internal electrical heating element 9 may be used. In such an embodiment, temperature may be controlled by manipulating electrical current in the internal electrical heating element 9 circuit.
- the heat source 4 is external and may be used with a conduit 16, conductor, or the like.
- steam 18 may be created using an external boiler as the heat source 4 in one embodiment, then passed through a conduit 16 running through the vessel 1, wherein a conductive portion 16 of the conduit is submerged in the distillate 2.
- the temperature of the distillate 2 may be controlled by varying the amount of steam 18 produced by the boiler. Such control may be provided by valves or similar means that are not pictured.
- the temperature of the distillate 2 in the vessel 1 is brought up to a temperature of about 160° F for a period of up to 48 hours. This process simultaneously extracts wood derived compounds and acids, some of which are thought to be esterification catalysts.
- the temperature of the distillate is measured via a temperature sensor 5. Any known temperature sensor may be used.
- the temperature of the distillate 2 may be controlled by manually manipulating the heat source 4.
- an electronic temperature sensor is coupled 10 to a controller 7.
- the controller 7 may be configured to present an alert (e.g., flash a light, produce a sound, produce an electrical signal, transmit a text message, e-mail or other electronic communication, etc.) when the temperature of the distillate 2 is outside of a provided range.
- the controller 7 may be coupled to the heat source 4, in which case, the controller is configured to manipulate the heat source to keep the temperature of the distillate 2 within the provided range.
- Heating in accordance with the invention triggers the esterification of free volatile acids and alcohols in the distillate 2, while the headspace 3 provides for reflux within the vessel 1 allowing any weak acids to be rapidly extracted from the wood.
- These weak acids in combination with elevated temperatures, appear to help catalyze the esterification of free acids in the distillate per the Fischer process, which would otherwise take many years in traditional containers.
- the pressure inside the container may be measured by a pressure sensor 6.
- the pressure sensor 6 may be coupled to the controller 7.
- the pressure sensor may be configured to provide alerts if the pressure becomes too high.
- the pressure sensor may optionally be configured to communicate to open a release valve if the pressure is too high.
- the first distilled spirit mixture provided in step (i) is generally allowed to cool and transferred for processing with actinic light.
- the first distilled spirit mixture is contacted with actinic light in the range of 400nm to lOOOnm for a cumulative exposure of at least 2,280,000 lux hours to give an actinic light-treated distilled spirit.
- the actinic light process takes place in a container that allows light in the UV-
- the container is filled with the spirit to be processed and is also generally filled with wood as described in the previous step.
- glass carboys are used.
- the actinic light may come from a variety of sources including natural, synthetic, or a combination thereof. Generally, the exposure in this step will be at least 2,280,000 lux hours, but sometimes as high as 20,000,000 lux hours. In other embodiments, the total exposure is at least 1,000,000 lux hours, at least 1,500,000 lux hours, at least 2,000,000 lux hours, at least 2,500,000 lux hours, or at least 3,000,000 lux hours. Where very high concentrations of the chemical markers described herein are sought even greater exposures might be appropriate.
- the time period over which the actinic light process is conducted can and will vary over different embodiments.
- the total exposure to actinic light may range from about 100 hours to about 500 hours, from about 250 hours to about 750 hours, from about 500 hours to about 1000 hours, from about 750 hours to about 1250 hours, or from about 1000 hours to about 1500 hours.
- the total exposure to actinic light may range from about 12 hours to about 24 hours, from about 24 hours to about 48 hours, from about 48 hours to about 96 hours. If artificial lights are used that provide a very low lux value, time is increased proportionally to achieve the lux hour value.
- the actinic light process is conducted below the boiling point of the spirit. In some embodiments, this requires that the amount or duration of actinic light is controlled, for example, by exposing the spirit to light in a discontinuous manner, by cooling the spirits, by temporarily shielding the spirit from the actinic light, or by other methods for controlling temperature that are known in the art. This process may also be carried out under reflux to prevent the evaporation of volatile compounds.
- the actinic light processing is generally conducted at atmospheric pressures.
- the light processing step may accommodate higher or lower pressures.
- a tungsten halogen bulb is used to provide the actinic light.
- the bulb has an average light temperature of 2900°.
- the sprits are placed in clear containers where about 100 liters of spirit cover a square meter. The area is illuminated to about 190,000 lux with the light being toggled off and on in periods of 2-4 hours to reach a total exposure of 4,500,000 lux hours.
- Lux hours describes the light exposure in a given hour because it describes the total luminescence in a given time. Radiant flux measurements were unavailable because the data was not available.
- a distilled spirit is placed in a translucent jar that was kept in a greenhouse for 168 hours to achieve a total of approximately 4,200,000 lux hours.
- halogen bulbs are used to provide light to seventy jars. The lights are toggled on and off for three days to provide the total lux hours needed for the reaction.
- 500 W halogen bulbs are shined on both sides of a glass jar. The lights are toggled on and off for 14 hours to provide the total lux hours needed for the reaction.
- the sequential process further involves a temperature process conducted with the resulting mixture from Section A(ii).
- the actinic light-treated distilled spirit mixture is heated to maintain the temperature of the actinic light-treated distilled spirit mixture between about 140° F and about 170° F for a period of time ranging from about 12 hours to about 336 hours in a sealed vessel or under reflux such that evaporation of volatile compounds is prevented to produce a mature spirit.
- A(iii) may be followed by one or more additional actinic light or thermal processing steps.
- a second actinic light processing step may be conducted on the product obtained by the second thermal processing step.
- a third thermal processing step may also be utilized after a second actinic light processing step.
- the processes includes a further step of (d) of contacting the product of step (c) with wood and actinic light at a wavelength ranging from 400nm to lOOOnm for a cumulative exposure of at least 2,280,000 lux hours.
- the process further comprises the step (e) of contacting the product of step (d) with wood at a temperature between about 140° F and about 170° F for a period of time ranging from about 24 hours to about 336 to give a first distilled spirit mixture
- the sequential process may be repeated until a desired chemical marker profile is obtained.
- the sequential process begins with an unmature distilled spirit contacted with actinic light as described in Section (A)(ii) to form an actinic light-treated distilled spirit mixture.
- actinic light-treated distilled spirit mixture is treated thermally as described in Section (A)(i).
- the present disclosure provides a mixed batch process for producing a mature spirit.
- the process comprises (a) contacting a first unmatured distilled spirit with wood at a temperature between about 140° F and about 170° F for a period of time ranging from about 24 hours to about 336 to give a first distilled spirit mixture; (b) contacting a second unmatured distilled spirit with wood and actinic light at a wavelength ranging from 400 nm to 1000 nm for a cumulative exposure of at least 2,280,000 lux hours to give a second distilled spirit mixture; and (c) mixing the first and second distilled spirit mixtures to produce the mature spirit.
- Step (a) of the process is conducted as described in Section (A)(i).
- the resulting first distilled spirit mixture is not reacted with light.
- a second unmatured distilled spirit mixture is treated with actinic light as described in Section (A)(ii).
- the resulting second distilled spirit mixture is not treated by the thermal processing step of Section (A)(i). Instead, the first distilled spirit mixture and the second distilled spirit mixture are mixed together.
- the first distilled spirit mixture and the second distilled spirit mixture may be mixed in any ratio without limitation. In one embodiment, the ratio ranges between about 70:30 and about 30:70 of the first distilled spirit mixture to the second distilled spirit mixture. In particular embodiments, the ratio of the first distilled spirit mixture and the second distilled spirit mixture is about 70:30, about 65:35, about 60:40, about 55:45, about 50:50, about 45:55, about 40:60, about 35:65, or about 30:70. High concentration products may range from 99: 1 to 1:99, or, more preferably from a ratio of 95:5 to 5:95 of the first distilled spirit mixture to the second distilled spirit mixture.
- the mixture of the first distilled spirit mixture and the second distilled spirit mixture is generally allowed to react for at least 1 hour. Without being bound to any theory, it is believed that chemical reactions occur during this time period that enhance the flavor profile over the flavor profile of the separately produced first distilled spirit mixture and the second distilled spirit mixture.
- the present disclosure provides simultaneous process for producing a mature spirit.
- the process comprises contacting a unmatured distilled spirit with wood and maintaining the temperature between about 140° F and about 170° F for a period of time ranging from about 12 hours to about 336 hours, and at the same time, contacting the unmatured distilled spirit with actinic light at a range of 400 nm to 1000 nm for a cumulative exposure of at least 2,280,000 lux hours to give a mature spirit.
- Thermal processing is conducted as described in Section (A)(i).
- Actinic light exposure is as described in Section (A)(ii).
- the disclosure provides a process for producing a spirit having characteristics of FIGs. 5 or 6, as described herein.
- the process comprises (a) obtaining a marker concentration of an ester in a target matured distilled spirit thereby giving a target marker concentration, such as ethyl decanoate, as shown in FIGs. 5 or 6, (b) contacting an unmatured distilled spirit with wood and processing as described in Sections A-C to form a distilled spirit mixture, measuring the marker concentration of the distilled spirit mixture, and (d) processing the distilled spirit mixture as described in Sections A-C until the marker concentration of the distilled spirit mixture reaches the target marker concentration.
- a target marker concentration such as ethyl decanoate
- the chemical marker concentration of the distilled sprit mixture may be compared to the target marker concentration in order to determine if heating and/or actinic light treating steps as described in Sections A-C can be discontinued. When the target concentration is not met, heating and/or light treatment steps are repeated.
- the method provides a tunable process for producing a distilled spirit having characteristics associated with, for example, FIGs. 5 or 6.
- the chemical marker associated with a matured distilled spirit may be ethyl decanoate.
- the process disclosed above is not limited to ethyl decanoate, but can be any other ester that has higher concentrations in a matured distilled spirit as compared to an unmatured distilled spirit.
- Esters are ideal markers for a heat process because the heat process excels at forming esters as opposed to other semi-volatile compounds like sinapaldehyde.
- Markers for the process include, but are not limited to ethyl decanoate, ethyl dodecanoate, ethyl octanoate, ethyl butyrate, and ethyl hexadecanoate.
- volatile esters can be used as chemical markers. But, semi-volatiles are preferred because they behave more predictably during processing.
- GCMS Gas Chromatography Mass Spectrometry
- FIG. 1 shows the semi- volatile fingerprint of an un-aged pot distilled rum. This is largely defined by a lack of activity for compounds having a retention time ranging from 5 to 30 minutes. Noteworthy characteristics include, but are not limited to the starting height of peak 1 corresponding to acetyl, peak 2 corresponding to ethyl decanoate, and peak 3 corresponding to ethyl dodecanoate. The absence of a peak for sinapaldehyde, which is described further in later examples, is noteworthy. FIG. 1 also shows an absence of white noise in the chromatogram starting at the 6 minute retention time point.
- Concentration of ethyl acetate was measured by direct injection mass spectrometry. The concentration of ethyl acetate was shown to be about 110,000 ⁇ g/L.
- FIG. 2 illustrates a semivolatiles profile characteristic of 32 year aged pot distilled rums. Key characteristics include the high acetal spike (peak 1) the high ethyl decanoate spike (peak 2) the high ethyl dodecanoate spike (peak 3) and the high sinapaldehyde spike (peak #4).
- peak 1 the high acetal spike
- peak 2 the high ethyl decanoate spike
- peak 3) the high ethyl dodecanoate spike
- peak #4 the high sinapaldehyde spike
- the relative heights of peaks 2, 3, and 4 in relation to each other is also important. Organoleptically maintaining this approximate ratio of peak heights to each other proved significant for creating the flavor characteristics associated with aged rum. Further noteworthy is the cluster of medium level peaks centered on the 15- minute mark (thought to be caramel additives and found to include significant amounts of glucose - this phenomena was also observed in known adulterated rum).
- Concentration of ethyl acetate was measured by direct injection mass spectrometry. The concentration of ethyl acetate was shown to be about 770,00( g/L. A more typical reading for ethyl acetate in a 32 year-old sample is 200,00( g/L.
- FIG. 3 shows the GCMS chromatogram of the resulting product.
- the GCMS shows promising (but inadequate) developments of acetyl (peak 1) ethyl decanoate (peak 2), ethyl dodecanoate (peak 3) and sinapaldehyde (peak 4). It also shows the development of some white noise. Overall this sample did not produce all of the organoleptic properties displayed in aged rum.
- Concentration of ethyl acetate was measured by direct injection mass spectrometry. The concentration of ethyl acetate was shown to be about 62,000 ⁇ g/L.
- the chromatogram shows some unexpected results along with major developments.
- the acetyl concentration (peak 1) unexpectedly fell to a concentration lower than that of either of its constituent parts (FIGs. 3 and 4). But, the acetal level was still elevated in comparison to the unprocessed rum (FIG. 1) by a factor of 1.75X.
- the furfural concentration (peak 5) and syringaldehyde concentration (peak 6) unexpectedly fell sharply correcting the overabundance of these compounds displayed in the actinic light-treated rum (FIG. 4).
- this product did produce the organoleptic properties displayed in aged rum, albeit a highly idiosyncratic aged rum. It did not display any of the extreme bitterness found in the actinic light reacted rum (FIG. 4), or the thinness of flavor displayed in the temperature treated rum (FIG. 3). It was observed that the peak heights of ethyl decanoate, ethyl dodecanoate, and sinapaldehyde were all elevated and had come closer to aligning than had been possible in either the heat-treated product or the actinic light-treated product alone. Therefore the mixture of the two products had produced a final product that approached meeting all of the key chemical markers outlined in our definition of a mature spirit.
- Concentration of ethyl acetate was measured by direct injection mass spectrometry. The concentration of ethyl acetate was shown to be about 170,00( g/L.
- FIG. 6 shows the GCMS chromatogram from a rum sample that has been processed with both heat and light in accordance with Example 6. It shows some unexpected results along with major developments.
- the acetyl concentration (peak 1) is as high as it is in the actinic light reacted rum (FIG. 4) more than 3X the starting concentration found in the unprocessed rum (FIG. 1) satisfying the acetyl chemical marker criteria for an aged spirit.
- the furfural concentration (peak 5) does not exhibit the overabundance displayed in the actinic light-treated rum (FIG. 4).
- the ethyl decanoate concentration (peak 2) shows a peak height 25% +/- higher than that found in the mixture of heat treated rum and actinic light reacted rum described in FIG. 5.
- the peak shows a relative concentration roughly 5X higher than the starting concentration in the unprocessed rum satisfying our minimum ethyl decanoate marker criteria for an aged spirit.
- the ethyl dodecanoate (peak 3) peak height was identical to that found in the mixture described in FIG. 5 and lines up almost identically with the ethyl decanoate concentration.
- the sinapaldehyde (peak 4) fell slightly from the light/heat mixture rum described in FIG.
- Concentration of ethyl acetate was measured by direct injection mass spectrometry. The concentration of ethyl acetate was shown to be about 59,00( g/L.
Abstract
Description
Claims
Priority Applications (8)
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MX2016008840A MX2016008840A (en) | 2014-01-10 | 2015-01-12 | Method for rapid maturation of distilled spirits using light and heat processes. |
CN201580003971.4A CN106103680B (en) | 2014-01-10 | 2015-01-12 | Ripe method is quickly made using the Spirit that light and heat is handled |
NZ721673A NZ721673A (en) | 2014-01-10 | 2015-01-12 | Method for rapid maturation of distilled spirits using light and heat processes |
JP2016563895A JP6488319B2 (en) | 2014-01-10 | 2015-01-12 | Rapid maturation of distilled liquor using light and heat treatment |
AU2015204533A AU2015204533B2 (en) | 2014-01-10 | 2015-01-12 | Method for rapid maturation of distilled spirits using light and heat processes |
CA2935162A CA2935162C (en) | 2014-01-10 | 2015-01-12 | Method for rapid maturation of distilled spirits using light and heat processes |
EP15735279.0A EP3092295A4 (en) | 2014-01-10 | 2015-01-12 | Method for rapid maturation of distilled spirits using light and heat processes |
IL246657A IL246657B (en) | 2014-01-10 | 2016-07-07 | Method for rapid maturation of distilled spirits using light and heat processes |
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JP (1) | JP6488319B2 (en) |
CN (2) | CN106103680B (en) |
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CA (1) | CA2935162C (en) |
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DE102022123814A1 (en) | 2022-09-16 | 2024-03-21 | Kurpfalz Distillers GmbH | Process for maturing a spirit drink |
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JP6846811B2 (en) * | 2018-03-07 | 2021-03-24 | 国立研究開発法人森林研究・整備機構 | Alcoholic beverages made from lignocellulose, a tree material, and their manufacturing methods |
CN108504478A (en) * | 2018-04-02 | 2018-09-07 | 蓬莱市沃林橡木桶有限公司 | A kind of process for beer production |
JP2021522856A (en) * | 2018-05-02 | 2021-09-02 | ロスト スピリッツ テクノロジー エルエルシー | High-speed aging method of distilled liquor using light and heat process |
IL260160A (en) * | 2018-06-19 | 2018-11-29 | Edvy Matan | Hyper aging system and method |
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- 2015-01-12 AU AU2015204533A patent/AU2015204533B2/en not_active Ceased
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CN110713892A (en) | 2020-01-21 |
JP2017501750A (en) | 2017-01-19 |
CN106103680A (en) | 2016-11-09 |
AU2015204533B2 (en) | 2018-11-08 |
CN106103680B (en) | 2019-11-15 |
NZ721673A (en) | 2022-07-29 |
JP6488319B2 (en) | 2019-03-20 |
AU2015204533A1 (en) | 2016-07-14 |
MX2016008840A (en) | 2017-04-10 |
EP3092295A1 (en) | 2016-11-16 |
IL246657A0 (en) | 2016-08-31 |
IL246657B (en) | 2020-05-31 |
CA2935162C (en) | 2022-03-22 |
CA2935162A1 (en) | 2015-07-16 |
EP3092295A4 (en) | 2017-09-20 |
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