CN106103680B - Ripe method is quickly made using the Spirit that light and heat is handled - Google Patents

Ripe method is quickly made using the Spirit that light and heat is handled Download PDF

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Publication number
CN106103680B
CN106103680B CN201580003971.4A CN201580003971A CN106103680B CN 106103680 B CN106103680 B CN 106103680B CN 201580003971 A CN201580003971 A CN 201580003971A CN 106103680 B CN106103680 B CN 106103680B
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China
Prior art keywords
wine
hours
ripe
spirit
light
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CN201580003971.4A
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Chinese (zh)
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CN106103680A (en
Inventor
布莱恩·亚历山大·戴维斯
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Lost Distillery Co Ltd
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Lost Distillery Co Ltd
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Priority to CN201911226560.8A priority Critical patent/CN110713892A/en
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/12Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
    • C12H1/16Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
    • C12H1/165Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation by irradiation
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12GWINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G3/00Preparation of other alcoholic beverages
    • C12G3/04Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs
    • C12G3/06Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs with flavouring ingredients
    • C12G3/07Flavouring with wood extracts, e.g. generated by contact with wood; Wood pretreatment therefor
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/12Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
    • C12H1/16Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
    • C12H1/18Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation by heating

Abstract

The present invention provides for quickly producing the improvement system and method with the Spirit of feature relevant to the quite long ripe technique of wine.This method includes contacting timber in a heated condition with ripe Spirit is not made, and contact obtained thermally treated wine with actinic light.Embodiment the present invention provides light and heat light processing Continuous maching wine is passed through.The present invention also provides by thermally treated wine with the embodiment to obtain making the feature of ripe wine is individually mixed with the wine of light processing.

Description

Ripe method is quickly made using the Spirit that light and heat is handled
Cross reference to related applications
This application claims the priority for the United States serial 14/152,915 submitted on January 10th, 2014, the U.S. Shens It is please incorporated into this by reference of text.
Technical field
Technical field are as follows: Food Chemistry and other consumer goods.
Background technique
According to some reports, the mankind have the history of the almost quincentenary ageing Spirit in cootle.Although There is the experience of billions of people-hours, but does not understand the countless chemical reaction for leading to the flavor of cootle ageing wine completely yet. Wine derives its unique feature when being stored in cootle at any time, is partly due to the generation and presence of ester.Ester is It is bonded by acid molecule with alcohol molecular chemistry to form the compound that noval chemical compound generates, usually there is pleasant fragrance and taste Road.The process referred to as " is esterified ".Other than esterification, the wine of cootle ageing also passes through other processes, including from wooden Aroma compound is extracted in container (for example, generally existing oak barrel), and derives additional feature.These processes are not necessarily It is separated or unique, but can interact with each other and interact.
Traditionally, produce cootle ageing Spirit include carboxylic esterification, phenolic acid esterification and including phenolic acid and carboxylic The formation of the complex ester of acid.Carboxylate leads to fruit aroma and taste in Spirit.Carboxylic acid precursor's acid derives from fermentation process In yeast and bacterium.In case of organic substance has been used in the container of these reactions, then these substances also will affect this Process.For example, carboxylic acid precursor's acid also derives from the rubber found in the liner of bucket when using the oak barrel burnt or toasted The thermal decomposition of the wooden polymer --- hemicellulose.Carboxylic acid precursor's acid mainly results in the " smell substance (off of Spirit flavors)".In addition, be similar to solvent " smell substance " common deficiency be by ethyl acetate in making ripe wine Accumulation and generate.Smell substance is the various flavoursome or fragrant compound being present in wine, usually by appreciation household Colourful term (for example, " sulfur smoke ", " solvent taste ", " meat flavour ", " tart flavour ", " metallic taste ", " vegetables taste " etc.) is retouched It states.Phenolic aldehyde also plays a significant role in generating the fragrance for being similar to vanilla, pipe tobacco and cigarette.Phenolic aldehyde is mainly derived from bucket The oak polymer of the thermal decomposition found in liner.Complex ester leads to honey fragrance complicated in Spirit.Complex ester usually produces It is born from the chemical reaction of both carboxylic acid and phenolic acid/aldehyde and alcohol during in bucket or other containers.
The esterification of the Fischer (Fischer) of fatty acid and alcohol is chemical reaction that is a kind of well-known and generalling use.Allusion quotation The lab process of type includes in the presence of acid catalyst heating the solution of fatty acid and alcohol under reflux.It is set in laboratory In setting, strong acid (for example, sulfuric acid) is generallyd use as catalyst, but this may be sensitive to strong acid and usual with other functional groups Forbid the wine brewing process of chemical addition agent incompatible.It has long been known that Fischer esterification can also using weak acid catalyst come It completes, but this is using relatively slow reaction rate as cost.When the ripe period use of wine in Spirit is burnt or is toasted Oak barrel when, weak acid may be extracted gradually from the organic substance in bucket wall.It is catalyzed using the weak acid from bucket Agent usually requires the several years to accumulate ester, although having been observed that under warmer environment (that is, normal big lower than 120 °F Appropriate heating in gas condition and range) process can substantially speed up (from many decades to several years).The acceleration of this old model is old Wine is to increase from the evaporation of bucket as cost.Usually up to 50% product may be lost due to evaporation.
It is that the process of the astringent taste of color and " oak taste " and " smoke " is provided to Spirit that wood, which extracts,.Traditionally, this gives the credit to In tannic acid (polyphenol).It is interesting that we are not found the clear evidence of tannic acid to the analysis for making ripe wine.And on the contrary, we Phenol derived from countless less complicated wood is had found, such as sinapyladehyde and syringaldehyde.Unexpectedly demonstrate the extraction of these oaks Compound as the marker for monitoring following aging process be useful.
Had attempted to by relatively large range (for example, -2 between 10ATM;Referring to United States Patent (USP) public affairs 2013/0149423) number of opening recycles or changes pressure to accelerate the wine of Spirit ripe.These techniques do not generate and pass through biography usually The close enough product of the product that system means generate.Other environmental conditions are more aggravated for obtaining feature related with ripe flavor is made It wants.
Being esterified and extracting the wooden compound from cootle is some main anti-of the generation during the wine of Spirit is ripe It answers.Because these processes are run simultaneously, and are usually interacted with each other or are interdepended, and dependent on changing over time The substance and other conditions of its environment, so being still to obtain while deviation conventional method is very remote similar the result is that very Difficult.For example, quickly oak extracts the possibly time that can not provide the interaction of enough and cootle to obtain presence Some more delicate and complicated flavor in the wine of traditional ageing.Many losses in wine brewing are from generation final product High latency and product are from the evaporation in bucket.Reserve must be stored, usually in the environment of climate controlling, and And it is tested repeatedly during wine is ripe.However, it is difficult to predict market later for many years.The manufacturer for producing multi-product can not make It, which is invested, maximizes, and the potentially beneficial market opportunity can not be caught by producing very few manufacturer.
The consumer of Spirit is usually educated and has identification capability.Many people will refuse to consume non-orthodox school The product of taste is paid.Need such method, by this method can reach within the period significantly shortened with The relevant quality of the wine of traditional ageing and complexity, the preferably evaporation of reduction finished product and the accumulation for reducing ethyl acetate.
Summary of the invention
There is provided herein the methods for producing the Spirit with the ripe wine correlated characteristic of wine, this method comprises: (a) makes not Make ripe Spirit and timber about 140 °F to about 170 °F at a temperature of contact one section of about 24 hours to about 336 hours when Between, to obtain Spirit mixture;(b) make the Spirit mixture and timber and wavelength in 400nm to 1000nm range Interior actinic light contact reaches at least 2, and the cumulative exposure of 280,000 luxs hour is mixed with the Spirit for obtaining photochemical light processing Close object;And the Spirit mixture of the photochemical light processing (c) generated into step (b) provides heat to maintain about 140 °F to arrive About 170 °F about 12 hours to about 336 hours a period of time of temperature makes ripe wine to generate.
In yet another embodiment, the present invention provides for producing the method with the Spirit for making ripe wine feature, This method include (a) making first do not make ripe Spirit and timber about 140 °F to about 170 °F at a temperature of contact about 24 hours and arrive About 336 hours a period of time, to obtain the first Spirit mixture;(b) second is made not make ripe Spirit and timber and wave The actinic light contact grown within the scope of 400nm to 1000nm reaches at least 2, the cumulative exposure of 280,000 luxs hour, to obtain After-fractionating wine mixture;And (c) the first and second Spirits mixture is mixed to generate and make ripe wine.
Other features and aspect of the invention will provide in more detail herein.
Detailed description of the invention
Fig. 1 shows the GCMS chromatogram of untreated Rum sample.
Fig. 2 shows the GCMS chromatograms for the sample for having passed through ageing 32 years commercially available Rums of traditional ageing technology.
Fig. 3, which is shown, to be subjected to heating but being not subjected to the GCMS chromatogram of the Rum sample of actinic light according to embodiment 3.
Fig. 4 shows the GCMS chromatogram for being subjected to actinic light according to embodiment 4 but being not subjected to the Rum sample heated.
Fig. 5 shows the GCMS chromatogram of the Rum sample according to embodiment 5, which is subjected to heating The mixture of Rum and the Rum for being subjected to actinic light.
Fig. 6 shows the GCMS chromatogram for the Rum sample for having used both light and heat to handle according to embodiment 6.
Fig. 7 shows the wooden barrel for heat treatment, and wherein section shows the internal structure of this barrel.
Fig. 8 shows the sealing vessel for heat treatment, and wherein section shows the internal structure of the vessel.
Specific embodiment
The present invention relates to for producing the method with the Spirit for making ripe Spirit correlated characteristic.It is produced according to this method Spirit have many features relevant to the ripe Spirit of wine produced according to industrial standard, but its advantageously shortening when Between production in section, while eliminating evaporation problems and greatly reducing " smell substance " related with Excess ethyl acetate.Pass through Make not make ripe Spirit and contacted at elevated temperatures with timber and contact the wine with actinic light, wine can not reduced Shorten in the case where quality and makes ripe process.In particular, it was surprisingly found that method described herein is in one section significantly shortened The wine with chemical marker similar with 32 years old wine is produced in time.
As used herein, wine refers to arbitrary Spirit.In certain embodiments, which is based on sugarcane, base In cereal, based on fruit or based on the wine of American aloe, such as Rum (rum), Te Jila wine (tequila), mescal (mescal), whiskey (whiskey), brandy (brandy), gin tonic (gin) or combinations thereof.
As used herein, there is the Spirit of feature relevant to ripe Spirit is made to describe such wine, the wine Feature relevant to the wine according to industrial standard ageing is obtained by one or more chemical markers.For example, such mark Standard includes that ageing is more than 1,5,10,15,20,25 or 30 year a period of time in wooden barrel by wine.It is related to the Spirit for making ripe Feature may include taste, fragrance and alcoholic degree characteristic, feel as alcohol is sliding.
In history, use ethyl acetate concentration as the marker of ageing progress, wherein higher amount indicates longer wine The ripe time.But ethyl acetate itself is undesirable, and is added to a kind of mouthfeel for being equivalent to paint thinner and fragrance.This Outside, do not have usually better than ageing wine, Spirit by higher rating sample quite or in some cases with ageing wine There is high ethyl acetate concentration.Using modern technologies, the chemical composition for the wine being of great rarity can analyze.By using the number According to can choose chemical marker as the model for making ripe wine., it is surprising that these chemical markers are relative to acetic acid Ethyl ester concentration determines that the traditional measurement in time has advantage.Specifically, for modeling purpose, chemical marker as described herein is Preferably, because being different from ethyl acetate, these chemical markers facilitate desired flavor characteristics.
Surprisingly, it was found that one group of chemical marker can be associated with the flavor characteristic for making ripe wine, regardless of How is ethyl acetate concentration.Further, it is found that making the method that ripe period reduces ethyl acetate concentration.Because of ethyl acetate Mouthfeel be undesirable, so the discovery improve by this method manufacture wine flavor characteristics.In an embodiment In, ethyl acetate concentration decreases below the concentration of about 200,000 μ g/L.In another embodiment, ethyl acetate concentration In the range of about 50,000 μ g/L to about 170,000 μ g/L.
As used herein, there is the ripe Spirit of wine of feature relevant to ripe Spirit is made to describe such wine, Which give flavor similar with the wine with wooden barrel ageing many years on sense organ and aroma characteristics, and usually show containing spy The chemical profile of the key chemical marker of certainty ratio.
In one embodiment, the feature for making ripe wine can be that the concentration of one or more chemical markers increases. Especially there are three types of markers to be considered for determining that it is particularly useful for making ripe wine: sinapyladehyde, ethyl caprate and ethyl laurate. The ethyl caprate and ethyl laurate of low concentration are often found in not making ripe wine.Do not find sinapyladehyde usually in not making ripe wine.
In one embodiment, ripe wine is made to be characterized in that relative to not making ripe wine, ethyl laurate increase at least about 3 Times.In another embodiment, it makes ripe wine to be characterized in that relative to not making ripe wine, at least about 3 times of ethyl caprate increase.Increase The concentration added can be estimated by any method known in the art.
With relative scale (as estimated according to the peak height measured by GCMS), there are the wine of these three compounds usually to have There is desired flavor characteristic.In this regard, making ripe wine can also have the feature that as measured by GCMS, sinapyladehyde peak Higher than ethyl caprate and the peak height of ethyl laurate 80% and lower than its 200%.It is without wishing to be bound by any theory, it is believed that mustard seed It is super important that aldehyde concentration, which meets the wine for the organoleptic properties for making ripe wine for generation,.
In another embodiment, making ripe wine is such a wine, is generated and sinapyladehyde shown in fig. 5, capric acid second The substantially similar opposite peak height of the peak height of ester and ethyl laurate.As used herein, " substantially similar " refers to opposite peak height Difference is 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 be no more than 2%.In yet another embodiment, making ripe wine is such a wine, is generated and sinapyladehyde shown in fig. 5, ethyl caprate, ten The substantially similar opposite peak height of the opposite peak height of two acetoacetic esters and acetyl group.In a further embodiment, making ripe wine is this A kind of wine of sample, generate with sinapyladehyde shown in fig. 5, ethyl caprate, ethyl laurate, acetyl group and syringaldehyde opposite peak height Substantially similar opposite peak height.
In yet another embodiment, making ripe wine is such a wine, is generated and sinapyladehyde shown in fig. 6, capric acid second The substantially similar opposite peak height of the opposite peak height of ester and ethyl laurate.In yet another embodiment, making ripe wine is such one Kind wine, opposite peak height is substantially similar with sinapyladehyde shown in fig. 6, ethyl caprate, ethyl laurate and acetyl group for generation Opposite peak height.In yet another embodiment, making ripe wine is such a wine, is generated and sinapyladehyde shown in fig. 6, capric acid second Ester, ethyl laurate, acetyl group and syringaldehyde the substantially similar opposite peak height of opposite peak height.
Not making ripe Spirit is the wine for not obtaining marker relevant to ripe Spirit is made or feature.As described herein , " not making ripe Spirit " refers to that white wine or thick wine, and part make ripe wine, and condition is that this does not make ripe Spirit shortage Make certain features of ripe wine.As described herein, the alcohol content that ripe Spirit has at least 50 percents by volume is not made. In some embodiments, the alcohol content of ripe Spirit is not made in 50 percents by volume between 80 percents by volume.
As used herein, term " Spirit mixture ", which refers to, ripe any is distillating to do not make in ripe range from making Object.As used herein, term " distillate " refer to the liquid composition in vessel and may include do not make ripe Spirit, Make ripe Spirit or Spirit mixture.
Ripe Spirit is not made to contact in vessel with timber.In one embodiment, which evaporates as this is accommodated Out the vessel of object and provide.In such embodiments, which is such as oak barrel.It in other embodiments, can be with Timber is provided inside to reaction vessels, which is optionally made of timber.For example, sawdust can be added so that its submergence or Swim in the top of distillate.Timber is also used as the construction of the various structures in vessel and provides, including as baffle or packet Fill object.In other other embodiments, timber may include wood extractive and the characteristic designed for simulated logs Ortho acid (raw acids).In preferred embodiments, which is oak.
In each advantage of the invention, an advantage is without providing additional ingredient or acid to promote the process.Just For this, which does not use additive.It is not being bound by any particular theory, it is believed that process of the invention is fast from timber Speed extracts acid.These acid promote esterification process, without the additive except timber and in addition to not making ripe Spirit.
A. temperature and light processing that sequence carries out
One aspect of the present invention provides the method for making ripe wine using continuous temperature and light processing production.With regard to this Speech, method includes the following steps: (a) make not make ripe Spirit and timber about 140 °F to about 170 °F at a temperature of contact About 24 hours to about 336 hours a period of time, to obtain Spirit mixture;(b) make the Spirit mixture and timber And actinic light contact of the wavelength within the scope of 400nm to 1000nm reaches at least 2, the cumulative exposure of 280,000 luxs hour, To obtain the Spirit mixture of photochemical light processing;And the Spirit mixing of the photochemical light processing (c) generated into step (b) Object provides heat to maintain about 140 °F to about 170 °F about 12 hours to about 336 hours a period of time of temperature, is made with generating Ripe wine.
(i) the first heat treatment
In continuous processing as described herein, make not make ripe wine through heat-treated.In this regard, make not making ripe distillation Wine and timber about 140 °F to about 170 °F at a temperature of contact.In alternative embodiment, temperature is at about 140 °F to about 150 ° F, in the range of about 145 °F to about 150 °F, about 150 °F to about 160 °F or about 160 °F to about 170 °F.
Ripe Spirit will not be made to be converted to relevant to ripe wine is made Partial Feature (for example, as shown in Figure 3) When period required for Spirit mixture depends on the starting composition for not making ripe Spirit such as and technique progress The factors such as temperature.In some embodiments, it provides constant temperature about 12 hours of about 140 °F to about 170 °F to about 336 small When a period of time.In replaceable embodiment, constant temperature about 12 hours to about 24 of about 140 °F to about 170 °F are provided Hour, about 24 hours to about 48 hours, about 48 hours to about 96 hours, about 96 hours to about 168 hours, about 168 hours are to about 226 hours or about 226 hours to about 336 hours a period of time.
Heating carries out in the vessel of sealing or under reflux, to prevent the evaporation of volatile compound.In the present invention Different embodiments in, pressure in vessel can with and will change.In general, the internal pressure for accommodating the vessel of reactive component is climbed Rise to about 6 pounds/square inch (psi) of maximum value.The typical range of pressure in vessel, but can be between 2psi to 6psi Desired chemical reaction is still realized while changing the operating pressure to relieve stress and remaining less than 1psi.
In one embodiment, temperature is maintained about 168 hours to about 226 hours between about 140 °F to about 150 °F A period of time.
In another embodiment, temperature is maintained about 24 hours to about 72 hours between about 150 °F to about 160 °F A period of time.
In general, continuously applying heat at a given time period.But it is also possible to discrete at a given time period Mode provides heat, such as provides heat at certain intervals, as long as the time for providing heat adds up to the defined period.At this At the end of period, the first Spirit mixture is obtained.In the embodiment of the invention, pass through the first of heat treatment generation Spirit mixture further progress is reacted as described below.
Heat treatment can carry out in equipment as shown in Figure 7, and the figure shows a kind of possible in-built sections Figure.Vessel 1 can be wooden barrel.
In the embodiment depicted in fig. 8, section is shown in broken lines to disclose the alternatively possible inside structure of vessel 1 It makes, wherein vessel 1 can be rustless steel container.In this embodiment, timber 12 is used as and is immersed in distillate 2 or swims in Clast or plank on the top of distillate 2 provide.
For both Fig. 7 and Fig. 8, heat can be applied via distillate 2 of the heat source 4 into vessel 1.In an embodiment In, vessel are sealed under stress.In another embodiment, vessel are heated under reflux to prevent volatile compound Evaporation.Any method that sufficient heat is introduced to distillate, including internal electrical heating elements 9 can be used.Such In embodiment, temperature can be controlled by manipulating the electric current in 9 circuit of internal electrical heating elements.In replaceable embodiment In, heat source 4 is in outside, and can be used together with conduit 16, conductor etc..In one non-limiting example, it can adopt It uses external boiler to generate steam 18 as heat source 4 in one embodiment, steam is then made to pass through the conduit across vessel 1 16, wherein the thermal conduction portions 16 of the conduit are immersed in distillate 2.It in such embodiments, can be by changing by pot The amount for the steam 18 that furnace generates controls the temperature of distillate 2.Such control by valve or can be depicted without similar Device provides.
In one embodiment, the temperature that the temperature of the distillate 2 in vessel 1 is risen to about 160 °F, continues most 48 A period of time of hour.The process extracts compound and acid derived from timber simultaneously, and some of which is considered as catalyzing esterification Agent.In one embodiment, the temperature of distillate is measured by temperature sensor 5.Any of temperature can be used to pass Sensor.The temperature of distillate 2 can be controlled by manual manipulation heat source 4.In replaceable embodiment, electron temperature sensing Device couples 10 to controller 7.Controller 7 may be configured to when sending when except provided range of the temperature of distillate 2 Alarm (for example, glisten, make a sound, issuing electronic signal, transmission text information, Email or other electronic communications etc.). Optionally, controller 7 is coupled to heat source 4, and in this case, controller is configured for manipulation heat source so that distillate 2 Temperature be maintained at provided by range.
The esterification of free volatile acid and alcohol in triggered distillate 2 according to the present invention, and headspace 3 provides Reflux in vessel 1, to allow any weak acid of rapidly extracting from timber.It is combined with raised temperature, these weak acid Seem that the free acid for helping to be catalyzed in distillate is esterified according to Fischer process, and this will need many in conventional container Year.
Pressure in container can be measured with pressure sensor 6.Pressure sensor 6 is coupled to controller 7.Pressure Sensor may be configured to provide alarm if pressure becomes excessively high.If pressure sensor can be optionally configured to Hypertonia is then communicated to open relief valve.
(ii) photochemical light processing
Usually make the first Spirit mixture provided in step (i) cooling and shift for photochemical light processing.According to One embodiment of the invention contacts the first Spirit mixture with the actinic light within the scope of 400nm to 1000nm and reaches At least 2, the cumulative exposure of 280,000 luxs hour, to obtain the Spirit of photochemical light processing.
Photochemical light processing occurs in the container for allowing the light in UV- visible spectrum to pass through.The vessel filling has to be processed Wine, and usually also as described in above-mentioned steps filled with timber.In one embodiment, using carboy (glass carboy).Actinic light can come from a variety of sources, including natural, synthesis or combinations thereof.In general, exposure in this step Light will be at least 2,280,000 luxs hour, but sometime up to 20,000,000 lux hour.In other embodiments In, total exposure is at least 1,000,000 lux hour, at least 1,500,000 luxs hour, at least 2,000,000 Le gram This hour, at least 2,500,000 luxs hour or at least 3,000,000 luxs hour.When the sheet for pursuing very high concentration When chemical marker described in text, bigger exposure may be suitable.
Carry out photochemical light processing period can with and will be changed according to different embodiments.When use nature The total exposure of light time, actinic light can be at about 100 hours to about 500 hours, about 250 hours to about 750 hours, about 500 hours To in the range of about 1000 hours, about 750 hours to about 1250 hours or about 1000 hours to about 1500 hours.It is synthesized when using The total exposure of light time, actinic light can be at about 12 hours to about 24 hours, about 24 hours to about 48 hours, about 48 hours to about 96 In the range of hour.If using the artificial light of low-down lux value is provided, in order to reach lux one hour value, time To proportionally it increase.
Preferably, photochemical light processing lower than wine boiling point at a temperature of carry out.In some embodiments, this needs to control The amount of actinic light processed or duration, for example, by the way that wine is exposed to light in discontinuous manner, by passing through wine cooling Wine is temporarily covered to avoid actinic light, or by known in the art for controlling the other methods of temperature.The process The evaporation to prevent volatile compound can be carried out under reflux.
Although it is believed that pressure be not for photochemical light processing it is critical, but photochemical light processing usually under atmospheric pressure into Row.Light processing step is adapted to higher or lower pressure.
In a preferred embodiment, it is steeped using tungsten halogen lamp and actinic light is provided.The light bulb is averaged with 2900 ° Light temperature.Wine is placed in transparent vessel, wherein about 100 liters of wine cover one square metre.With cutting within 2-4 hours periods The light of closing and opening is changed to irradiate the region to about 190,000 luxs, to reach total exposure of 4,500,000 luxs hour Light.As used herein, lux hour describes the light exposure within given hour, because which depict within given time It is total shine.Since data can not obtain, so radiant flux measurement value can not obtain.
In another embodiment, Spirit is placed in the translucent bottle kept in the greenhouse 168 hours, to reach To about 4,200,000 luxs in total hour.
In another embodiment, light is provided to 70 bottles using the halogen bulb of 20 500W.Light switching is beaten It is open and close to continue three days, to provide reaction required total lux hourage.
In yet another embodiment, make the two sides of 500W halogen bulb irradiation vial.Light is switched and is opened and closed Continue 14 hours, to provide reaction required total lux hourage.
When photochemical light processing is completed, the wine mixture of resulting photochemical light processing is removed from light source.
(iii) the second heat treatment
Continuous processing further comprises the Temperature Treatment carried out to the gained mixture from the part A (ii).In this regard, The Spirit mixture of photochemical light processing is heated in the vessel of sealing or under reflux, so that the distillation of the photochemical light processing The temperature of wine mixture was maintained between about 140 °F to about 170 °F for about 12 hours to about 336 hours a period of time, with Just the evaporation of volatile compound is prevented to generate and make ripe wine.
The process being heat-treated to the wine of photochemical light processing carries out in a manner of described in the part A (i), and difference exists It is carried out in Spirit mixture of the process to the photochemical light processing generated according to the part A (ii).Advantageously, which causes The significant decrease of the ethyl acetate concentration generated during actinic light processing experimentally shows that it is reduced more than 60%.
(iv) optional to be further processed
Optionally, the wine that the generation of process described in the part A (iii) is partially arrived by A (i) then can carry out one or more A additional actinic light or heat treatment step.For example, the second light can be carried out to the product obtained by the second heat treatment step Change light processing step.Third heat treatment step can also be used after the second actinic light processing step.In an embodiment In, this method includes further step (d): making the product of step (c) with timber and wavelength in 400nm to 1000nm range Cumulative exposure of the interior actinic light contact up at least 2,280,000 luxs hour.In yet another embodiment, this method into One step includes step (e): make the product of step (d) and timber about 140 °F to about 170 °F at a temperature of contact about 24 hours and arrive About 336 hours a period of time, to obtain the first Spirit mixture.
In one embodiment, chemical marker map of the continuous processing needed for obtaining can be repeated.
(v) embodiment that sequence reverses
In yet another embodiment of the present invention, the continuous processing connects from as described in the part (A) (ii) with actinic light The ripe Spirit of not making of touching starts, to form the Spirit mixture of photochemical light processing.After this treatment, by photochemical light processing Spirit mixture be heat-treated as the part (A) (i) is described.These steps can be repeated until obtaining such as by described herein Chemical marker determine required flavor characteristics.
B. batch process is mixed
In another embodiment, the present invention provides for producing the mixing batch process for making ripe wine.In the implementation In scheme, the technique include (a) making first do not make ripe Spirit and timber about 140 °F to about 170 °F at a temperature of contact about 24 hours to about 336 hours a period of time, to obtain the first Spirit mixture;(b) second is made not make ripe Spirit and wood The accumulation of actinic light contact up at least 2,280,000 luxs hour of material and wavelength within the scope of 400nm to 1000nm exposes Light, to obtain after-fractionating wine mixture;And (c) the first and second Spirit mixtures are mixed to generate and make ripe wine.
The step of technique (a), carries out as described in the part (A) (i).Resulting first Spirit mixture not with light Reaction.Individually, as described in the part (A) (ii), ripe Spirit mixture is not made with photochemical light processing second.Resulting second The heat treatment step that Spirit mixture does not pass through the part (A) (i) is handled.On the contrary, by the first Spirit mixture and After-fractionating wine mixture mixes.
First Spirit mixture can be mixed without restriction with arbitrary proportion with after-fractionating wine mixture.At one In embodiment, the ratio of the first Spirit mixture and after-fractionating wine mixture is in about 70:30 to the range of about 30:70 It is interior.In specific embodiments, the ratio of the first Spirit mixture and after-fractionating wine 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 product can be In the range of 99:1 to 1:99, alternatively, it is highly preferred that the ratio of the first Spirit mixture and after-fractionating wine mixture is 95:5 to 5:95.
React the first Spirit mixture with the mixture of after-fractionating wine mixture at least 1 hour.Not by appoint What theoretical limitation, it is believed that chemical reaction occurs during this period of time, relative to the first Spirit mixture individually generated with The flavor characteristics of after-fractionating wine mixture, increased response flavor characteristics.
C. the light and heat processing carried out simultaneously
In yet another embodiment, the present invention provides the methods carried out while making ripe wine for producing.In the reality Apply in scheme, this method include make not make ripe Spirit contacted with timber and keep the temperature at about 140 °F to about 170 °F it Between for about 12 hours to about 336 hours a period of time, and at the same time, make this do not make ripe Spirit with 400nm extremely Actinic light contact within the scope of 1000nm reaches at least 2, the cumulative exposure of 280,000 luxs hour, to obtain making ripe wine.At heat Reason is carried out as described in the part (A) (i).Actinic light exposure is carried out as described in the part (A) (ii).
D. ripe wine is made by measurement chemical marker production
In yet another embodiment, the present invention provides for producing feature as described herein with Fig. 5 or Fig. 6 Wine method.This method, which includes (a) obtaining, makes the marker concentration of the ester in ripe Spirit in target, thus obtains such as Fig. 5 Or blip object concentration shown in fig. 6 (b) makes not make ripe Spirit and contacts with timber and such as such as ethyl caprate concentration It is handled described in the part A-C to form Spirit mixture, measures the marker concentration of the Spirit mixture, and (d) the Spirit mixture is handled as described in the part A-C, until the marker concentration of the Spirit mixture reaches target mark Will object concentration.
Once obtaining the chemical marker concentration of Spirit mixture, it can be compared with blip object concentration Compared with to determine whether to stop heating and/or actinic light processing step as described in the part A-C.Work as miss the mark When concentration, Repeat-heating and/or light processing step.Therefore, this method provides have and such as Fig. 5 or Fig. 6 phase for producing The adjustable process of the Spirit of the feature of pass.In one embodiment, chemical marker relevant to ripe Spirit is made can To be ethyl caprate.However, method disclosed above is not limited to ethyl caprate, and can be compared with not making ripe Spirit With any other ester of higher concentration in making ripe Spirit.Because heat treatment tends to form ester rather than other are partly waved Hair property compound such as sinapyladehyde, so ester is the ideal marker of heat treatment.
The marker of the method includes but is not limited to ethyl caprate, ethyl laurate, ethyl caprilate, ethyl butyrate and ten Six acetoacetic esters.In some embodiments, volatility ester may be used as chemical marker.However, because half volatile matter is being handled The performance of period is more predictable, so half volatile matter is preferred.
Example
Instrument
Using with Rui Sitaikang (Restek) chromatographic column-Rxi-5Sil MS, 30 meters, 0.24mm ID, 0.24umdf- Shimadzu (Shimadazu) gas chromatography-mass spectrometry (GCMS) QP2010 type obtain gaschromatographic mass spectrometry data.Program Condition is as follows:
Table 1: analytical line 1
Pre- solvent rinsing times :1
(rear) solvent rinse number :5
Sample rinsing times :1
Velocity of plunger (suction) : in
Viscous compound inhales the sample time :5.0sec
Velocity of plunger (injection) : it is high
Syringe insertion speed : it is high
Injection pattern Normally
Pumping number :3
The injection port residence time :10.0sec
Terminal air gap : it is no
Plunger washing speed : it is high
Wash volumes :6uL
Syringe suction position -2.0mm
Syringe injection position :0.0mm
Solvent selection : whole A, B, C
Table 2:GC parameter
Table 3: Temperature of Warm Case program
Rate Temperature (DEG C) Retention time (min)
35.0 5.00
16.00 300.0 1.44
Table 4:MS parameter
Ion source temperature :220.00℃
Interface temperature :280.00℃
The solvent mute time :1.80min
Detector gain mode : it is opposite
Detector gain :0.20kV
Threshold value :500
Initial time :1.80min
Terminate the time :23.00min
ACQ mode : scanning
Event time :0.50sec
Scanning speed :1000
Originate m/z :35.00
Terminate m/z :500.00
Comparative example 1: fresh Rum
The fresh Rum sample for not making ripe pot distillation is analyzed by GCMS.Fig. 1 shows the pot distillation of non-ageing Rum half volatile finger-print.This is mainly the activity of the compound by retention time within the scope of 5 to 30 minutes Lack and determine.Noticeable feature includes but is not limited to the peak 1 for corresponding to acetyl group, the peak 2 corresponding to ethyl caprate And the starting altitude at the peak 3 corresponding to ethyl laurate.The missing at the peak of sinapyladehyde is it is noted that it is in reality below It applies in example and further describes.Fig. 1 also shows the missing of the white noise in chromatogram since 6 minutes retention time points.
The concentration of ethyl acetate is measured by direct-injection MS method.The concentration for showing ethyl acetate is about 110,000 μ g/ L。
Comparative example 2: pass through the Rum of traditional aging process ageing 32 years
It is also analyzed by GCMS and has passed through ageing 32 years commercially available Rum samples of traditional aging process.Fig. 2 Show half volatile matter spectrum signature of the pot distillation Rum of ageing in 32 years.Crucial feature includes high acetal spike (peak 1), height Ethyl caprate spike (peak 2), high ethyl laurate spike (peak 3) and high sinapyladehyde spike (peak #4).Peak 2,3 and 4 is relative to that This relative altitude is also important.On sense organ, it was demonstrated that maintain this approximate ratio of the peak height relative to each other for It is meaningful to generate flavor characteristics relevant to the Rum of ageing.It is further noted that centered on 15 minutes labels Medium level peak group (be considered as caramel additive, and find it includes the glucose of significant quantity --- this phenomenon also exists It is observed in known adulterated Rum).
The key difference of the non-ageing Rum and 32 years Rums that can determine in half volatile matter chromatogram is included in aobvious Significant raised ethyl caprate is shown and ethyl laurate level (is found, it is characterised in that relatively low in white rum Peak value) peak beside there are sinapyladehydes (not to find in white rum).Finally, significant " white noise " layer (permitted by representative The complex mixture of most volatile compounds) appear in 32 years Rums chromatogram bottom, and in the Lang Mu of non-ageing It is not present in wine.
The concentration of ethyl acetate is measured by direct-injection MS method.The concentration for showing ethyl acetate is about 770,000 μ g/ L.The more typical reading of ethyl acetate is 200,000 μ g/L in 32 years samples.
Comparative example 3: the technique only heated
The Rum for the heavy pot distillation for not carrying out other processing is added in stainless cylinder of steel, and is mixed with the oak floor burnt Merging is heated between 150 °F to 170 °F.It keeps the temperature within the scope of this 48 hours.Fig. 3 shows the GCMS of products therefrom Chromatogram.The GCMS shows acetyl group (peak 1), ethyl caprate (peak 2), ethyl laurate (peak 3) and sinapyladehyde (peak 4) Promising (but insufficient) development.Also show the development of some white noises.On the whole, which does not generate The whole organoleptic properties shown in the Rum of ageing.The mouthfeel and fragrance of the sample are light singularly, and lack in 32 years samples The smoke found in product/woody flavour mouthfeel.From quality, it is unable to satisfy two key chemical marks of ageing Rum production Object standard.As it can be seen, white-noise level is lower.Ethyl laurate (peak 3) and sinapyladehyde (peak 4) does not reach and capric acid The similar peak height of ethyl ester (peak 2).
The concentration of ethyl acetate is measured by direct-injection MS method.The concentration for showing ethyl acetate is about 38,000 μ g/ L。
Comparative example 4: the only technique of actinic light
The Rum for the heavy pot distillation for not carrying out other processing is placed on to the flint of sealing together with the oak floor burnt In vial, and place 30 days in the greenhouse.The sample is not subjected to any heat treatment.The sample is analyzed by GCMS.The GCMS Show the significant development of acetyl group (peak 1), ethyl caprate (peak 2), ethyl laurate (peak 3) and sinapyladehyde (peak 4).It is also aobvious Show the development for making expected white-noise level in ripe wine.It is shown in the Rum of ageing however, the sample is not generated Organoleptic properties.It is extremely bitter.From quality, it is unable to satisfy a key chemical marker standard of ageing wine production.Mustard Sub- aldehyde (peak 4) is high.According to conjecture, the extreme horizontal of sinapyladehyde and observe some other and abnormal high peak (including Furfural (peak 5) and syringaldehyde (peak 6)) partly lead to the bitter taste together.
The concentration of ethyl acetate is measured by direct-injection MS method.The concentration for showing ethyl acetate is about 62,000 μ g/ L。
Embodiment 5: heating and photochemical light technology in batches is mixed
The Rum for the heavy pot distillation for not carrying out other processing is added in stainless cylinder of steel, and is mixed with the oak floor burnt Merging is heated between 150 °F to 170 °F.It keeps the temperature within the scope of this 48 hours.Individually, other processing will not be carried out The Rum of heavy pot distillation be placed on together with the oak floor burnt in the flint glass bottle of sealing, and place in the greenhouse 30 It.Then the product of the product of heat treatment and light processing is mixed, its ratio be 60% heat-treated products and The Rum of 40% photochemical light processing.React the mixture 24-48 hours.After the time period, institute is analyzed by GCMS Obtain product.Fig. 5 shows GCMS chromatogram.The chromatogram shows some unexpected results and important development. Acetyl group concentration (peak 1) unexpectedly decreases below the concentration (Fig. 3 and Fig. 4) of its any component part.But acetal is horizontal 1.75 times are still increased compared to untreated Rum (Fig. 1).Furfural content (peak 5) and cloves aldehyde concentration (peak 6) go out people's will Material ground sharply declines, and corrects for the excess (Fig. 4) of these compounds shown in the Rum of photochemical light processing.Ethyl caprate Concentration (peak 2) unexpectedly (and things turn out contrary to one's wishes ground) decreases below the level observed in any constituent component --- But the peak still maintains 3 times more than the initial concentration in untreated Rum, meets our lowest bids to ageing wine It is quasi-.Ethyl laurate (peak 3) is not influenced by product merging.Crucially, it is contemplated that found in the product of photochemical light reaction High peak (Fig. 4), sinapyladehyde (peak 4) decreases below expected concentration." white noise " is significant and unexpectedly reduces, The standard of ageing wine can not be fully met.Although the product can not fully meet some markers of 32 years wine, the product is true The organoleptic properties shown in ageing Rum are produced in fact, although a kind of very peculiar ageing Rum.It does not show The sense extremely bitter to the taste found in the Rum (Fig. 4) of photochemical light reaction or the display in the Rum (Fig. 3) of Temperature Treatment are shown Any one of thin mouthfeel.Observe that the peak height of ethyl caprate, ethyl laurate and sinapyladehyde all increases, and than single The closer alignment of the peak height that only heat-treated products or photochemical light processing product are likely to be breached.Therefore, the mixing of both products Object, which produces to approach, meets our final products to the whole key chemical markers summarized in the definition for making ripe wine.
The concentration of ethyl acetate is measured by direct-injection MS method.The concentration for showing ethyl acetate is about 170,000 μ g/ L。
Embodiment 6: the temperature and light processing that sequence carries out
The Rum for the heavy pot distillation for not carrying out other processing is added in stainless cylinder of steel, and is mixed with the oak floor burnt Merging is heated between 150 °F to 170 °F.It keeps the temperature within the scope of this 48 hours.Then by products therefrom with burn Oak floor is placed on together in the flint glass bottle of sealing, and is placed in front of 500W halogen bulb 3 days.70 vials are put It sets on the shelf surrounded by 20 beam light in total.Light was switched with 2-4 hours periods and is opened and closed, is risen to prevent defervescence.So Products therefrom is placed in stainless cylinder of steel afterwards, and is mixed and heated between 150 °F to 170 °F with the oak floor burnt.It will Temperature is kept for 48 hours in the range.Products therefrom is analyzed with GCMS.
Fig. 6 shows the GCMS chromatogram for the Rum sample for having used both light and heat to handle according to embodiment 6.It is aobvious Show some unexpected results and important development.With the Rum of light and heat light processing shown in Fig. 5 Mixture is different, acetyl group concentration (peak 1) with it is equally high in the Rum of photochemical light reaction (Fig. 4), be untreated bright 3 times or more of the initial concentration found in nurse wine (Fig. 1) meet the acetyl group chemical marker standard for being directed to ageing wine.Furfural Concentration (peak 5) does not show the excess shown in the Rum (Fig. 4) of photochemical light processing.Ethyl caprate concentration (peak 2) is aobvious Show that the peak height found in the mixture than heat treatment Rum and photochemical light reaction Rum shown in fig. 5 is high by 25% +/- peak height.The peak shows the relative concentration of about 5 times of initial concentrations in untreated Rum, meets us To the minimum ethyl caprate marker standard of ageing wine.It is sent out in ethyl laurate (peak 3) peak height and mixture shown in fig. 5 Existing peak height is identical, and almost arranges identically as ethyl caprate concentration.Sinapyladehyde (peak 4) is mixed with light heat shown in Fig. 5 Object Rum is closed compared to slightly declining, with ethyl caprate (peak 2) and ethyl laurate (peak 3) close alignment, satisfaction makes peak 2,3 and 4 substantially aligned unapproachable chemical marker standards.Since the improved technique meets the chemistry mark of ageing wine production Will object standard, therefore " white noise " peak also increases (compared to the mixture product shown in Fig. 5).As read desired by chromatogram , which produces the organoleptic properties shown in ageing Rum really.It does not show in the bright of photochemical light reaction The sense extremely bitter to the taste found in nurse wine (Fig. 4) or any one of the thin mouthfeel shown in the Rum (Fig. 3) of Temperature Treatment. It observes, the peak height of ethyl caprate, ethyl laurate and sinapyladehyde all increases, and with one kind in heat-treated products or photochemical The mode for being impossible to reach in light processing product or in the mixture (showing in Fig. 5) of even the two is substantially aligned.The work Skill has successfully met us to the whole key chemical markers summarized in the definition for making ripe wine, has well solved industry The problem of upper " in bucket 30 years ".It is unexpected and advantageously causes the significant decrease of ethyl acetate concentration, experiments have shown that with dividing Technique (Fig. 5) is criticized compared to reduction more than 60%.The technique will not lead to the finished product that expection will occur in traditional bucket ageing Evaporation.The finished product not only simulates the key point object ratio of traditional ageing product, and eventually by shorten make the ripe time, It eliminates evaporation and reduces ethyl acetate and improve technique.
The concentration of ethyl acetate is measured by direct-injection MS method.The concentration for showing ethyl acetate is about 59,000 μ g/ L。

Claims (22)

1. a kind of produce the method for making ripe wine comprising:
(a) make not make ripe Spirit and timber about 140 °F to about 170 °F at a temperature of contact it is about 24 hours to about 336 small When a period of time, to obtain Spirit mixture;
(b) the Spirit mixture is contacted with the actinic light of timber and wavelength within the scope of 400nm to 1000nm to reach The cumulative exposure of few 2,280,000 luxs hour, to obtain the Spirit mixture of photochemical light processing;And
(c) the Spirit mixture of the photochemical light processing generated into step (b) provides heat to maintain about 140 °F to about 170 ° About 12 hours to about 336 hours a period of time of the temperature of F makes ripe wine to generate.
2. according to the method described in claim 1, wherein described do not make ripe Spirit selected from sugarcane, cereal wine, Eaux-De-Vie Or mescal.
3. according to the method described in claim 1, wherein described do not make ripe Spirit selected from Rum, Te Jila wine, Mace Karr wine, whiskey, brandy and gin tonic.
4. according to the method described in claim 1, the wherein increase made ripe wine and be characterized in that sinapyladehyde.
5. according to the method described in claim 1, wherein the ripe wine of wine is characterized in that sinapyladehyde, ethyl laurate and capric acid The increase of ethyl ester.
6. according to the method described in claim 1, wherein the ripe wine of wine is characterized in that as passed through gas chromatography combined with mass spectrometry Measured by instrument GCMS, the amount of sinapyladehyde, ethyl laurate and ethyl caprate is consistent.
7. according to the method described in claim 1, wherein described make ethyl acetate concentration of the ripe wine with about 59,000 μ g/L.
8. according to the method described in claim 1, wherein step (a) and (c) are tieed up at a temperature of about 140 °F to about 150 °F Hold about 168 hours to about 226 hours a period of time.
9. according to the method described in claim 1, wherein step (a) and (c) are tieed up at a temperature of about 150 °F to about 160 °F Hold about 24 hours to about 72 hours a period of time.
10. according to the method described in claim 1, wherein this method further comprises:
(d) it contacts the product of step (c) with the actinic light of timber and wavelength within the scope of 400nm to 1000nm and reaches at least 2, The cumulative exposure of 280,000 luxs hour.
11. according to the method described in claim 10, wherein this method further comprises:
(e) make the product of step (d) and timber about 140 °F to about 170 °F at a temperature of contact about 24 hours to about 336 hours A period of time.
12. in step (b), the actinic light is synthesis light according to the method described in claim 1, wherein, then actinic light Total exposure is in the range of about 12 hours to about 96 hours.
13. a kind of produce the method for making ripe wine comprising:
(a) make not making ripe Spirit and contact with the actinic light of timber and wavelength within the scope of 400nm to 1000nm to reach at least The cumulative exposure of 2,280,000 luxs hour, to obtain the Spirit mixture of photochemical light processing;
(b) make the Spirit mixture of the photochemical light processing and timber about 140 °F to about 170 °F at a temperature of contact about 24 Hour arrives about 336 hours a period of time, makes ripe wine to generate.
14. according to the method for claim 13, wherein described do not make ripe Spirit selected from sugarcane, cereal wine, fruit Wine or mescal.
15. according to the method for claim 13, wherein described do not make ripe Spirit selected from Rum, Te Jila wine, wheat This karr wine, whiskey, brandy and gin tonic.
16. according to the method for claim 13, wherein the increase made ripe wine and be characterized in that sinapyladehyde.
17. according to the method for claim 13, wherein the ripe wine of wine is characterized in that sinapyladehyde, ethyl laurate and the last of the ten Heavenly stems The increase of acetoacetic ester.
18. according to the method for claim 13, wherein in step (a), the actinic light is synthesis light, then actinic light Total exposure in the range of about 12 hours to about 96 hours.
19. according to the method for claim 13, wherein by step (b) about 140 °F to about 150 °F at a temperature of maintain about 168 hours to about 226 hours a period of time.
20. according to the method for claim 13, wherein by step (b) about 150 °F to about 160 °F at a temperature of maintain about 24 hours to about 48 hours a period of time.
21. according to the method for claim 13, this method further comprises:
(c) it contacts the product of step (b) with the actinic light of timber and wavelength within the scope of 400nm to 1000nm and reaches at least 2, The cumulative exposure of 280,000 luxs hour.
22. according to the method for claim 21, this method further comprises:
(d) make the product of step (c) and timber about 140 °F to about 170 °F at a temperature of contact about 24 hours to about 336 hours A period of time.
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