CN109722358A - A kind of method of preparation and the use oak barrel preservation of ice wine - Google Patents

Abstract

The invention belongs to the preparation of ice wine and method for preserving, and in particular to a kind of method of preparation and the use oak barrel preservation of ice wine.This method is selected by ice grape, cleaning, is crushed, enzymatic hydrolysis, juicing, inoculation, fermentation, pouring, lower glue, filtering, ageing, filtering, refined filtration, oak barrel storage.The present invention carries out 100% original juice fermentation using pure ice grape, the faint scent of fragrance and oak that the ice-wine of production has ice grape intrinsic, oak barreled ice-wine is remarkably improved oxidation resistance, and 2.2 times and 2.0 times are respectively increased than common ice-wine in Lipid-soluble antioxidative activity and Water-soluble antioxidant ability.Oak barreled store sth. in a cellar time ice-wine potassium rich in, receive, mineral elements, the especially Se content such as calcium, iron, zinc, copper, manganese, magnesium, selenium are higher by 300 times than common ice-wine.The present invention can establish ice-wine fermentation technique, oak barrel stores sth. in a cellar ageing, the integrated new technology of quality-improving, have significant social and economic benefit.

Description

A kind of method of preparation and the use oak barrel preservation of ice wine

Technical field

The invention belongs to the preparation of ice wine and method for preserving, and in particular to a kind of preparation of oak barreled ice wine and preservation side Method.

Background technique

For ice wine because sweet perfumes are diffused all around for its fragrance, the sweet surprise of mouthfeel is good, deeply attracts numerous consumers.Ice wine refers to grape Harvesting is postponed, when temperature makes grape keep certain time on branch lower than -7 DEG C, icing, harvesting is squeezed under icing condition, Fermentation, grape wine made of brew (do not allow additional sugar source) in process of production.Ice wine by color be divided into red ice-wine and White ice-wine.Worldwide, the Niagara area of Ontario, Canada is current ice wine foremost in the world The states such as producing region, followed by Germany, Australian and France, Hungary.In recent years, Liaoning Province, China Manchu Autonomous County of Juanren Huan The mountainous region Long Hu becomes domestic important ice grape production base.The mountainous region Huan Long Hu is situated at the foot of a hill and beside a stream, and height above sea level is low, mean sea level 380m, The cold wet miniclimate in unique region that suitable planting ice grape planting is formd by landform, river, lake, vegetation, soil property etc..Huan The mountainous region Long Hu winter is cold but does not dry, and the most hot moon (July and August) temperature on average is 23.1 DEG C, average annual temperature, average annual rainfall Ideal conditions needed for amount, soil property, average relative humidity etc. reach ice grape growth, production is rare in global range Suitable ice grape planting region.Exactly because the advantageous ecology in the mountainous region Huan Long Hu, geographical, climatic superiority, now distant The ice-wine annual output of the Manchu Autonomous County of Juanren Ning Sheng reaches 840 tons, accounts for 30% of Gross World Product or so, occupies world head Position.

In traditional ice-wine brewage process, the mode that ice grape postpones harvesting, GB/T 25504-2010 are generallyd use " when temperature makes grape keep certain time on branch lower than -7 DEG C, icing is harvested " is recorded in ice-wine, still, at me The Northeast, state, it is more that the mode of being prepared will lead to ice grape shattering, and grape branch is easy frostbite, influences the production of next year Amount.Therefore, this method is not particularly suited for the Northeast, China.

Oak barrel is the best ageing container of ice-wine.Oak tissue has the characteristics that porous, can slowly add The traditional aging process of fast grape wine, while the chemical combination such as tannin, lignin, vanillic aldehyde, Oak Lactone, eugenol contained in oak Substance can be dissolved in grape wine, these substances can make the color of grape wine is more stable, mouthfeel is more soft, fragrance more Coordinate.In addition, oak barrel wall is because having permeability, thus the clarity of grape wine can be improved.The kind of oak, the age of tree, growth Baking degree, oak barrel in environment, process using the factors influences grape wine such as length of time and access times Ageing effect.The grape wine that material quality and the excellent grape of maturity are brewed through excellent brew technique, then through oak barrel Ageing can become softer, mellow and full, big and fleshy.But this field is less to oak barreled ice wine quality comparison correlative study, especially It is that research of the oak barrel in terms of the ageing of ice wine is rarely reported.

Summary of the invention

To make up the deficiencies in the prior art, the present invention passes through VIDAL (Vidal Blanc) ice grape in the brewing process of ice wine It selects, clean, selected and ice-breaking juicing, enzymatic hydrolysis, juicing, inoculation, fermentation, pouring, lower glue, filtering, ageing, filtering, refined filtration, rubber Wooden barrel storage proposes a kind of method that ice grape quality keeps and promoted, while optimizing the brewing and ageing of ice-wine Technique improves the brewing technique of ice-wine from multi-angles such as active component detection, flavor tastes.

To achieve the above object, the present invention adopts the following technical scheme that,

(1) ice grape harvests

When vineyard nocturnal temperature is lower than -7 DEG C, the related one section of branch of ice grape fruit ear is cut, is suspended on Portugal nearby On grape frame, when nocturnal temperature reaches -10 DEG C--15 DEG C, ice Portugal is transported in night grape-picking fruit ear, and within 2 hours Grape processing workshop carries out selected；

(2) ice grape is selected and ice-breaking is squeezed the juice

The temperature in the selected workshop of ice grape is -5 DEG C--10 DEG C, it is selected to carry out artificial grain, and carry out immediately with ice-cold It squeezes, obtain inspissated juice from the crack of frost fruit and filters, obtain the ice grape juice that sugar content is up to 410-420g/L；

(3) saccharomycete activates

Since sugar content is too high in ice grape juice, fermentation reaction is difficult to start, therefore need to activate to yeast.At 20 DEG C Wild grape juice and ice grape juice are mixed with the ratio of 2:1, inoculation 0.4-0.5g/L saccharomycete is activated, and activation time is 48h, yeast cell number will reach 10 in activating solution⁸A/L.

(4) cold fermentation, cellar storage

Using activating solution obtained by step (3) as fermentation liquid, it is inoculated into ice grape juice and is led in the ratio of 5% (v/v) Fermentation, fermentation temperature are 15 DEG C, and the main fermentation time is 2-3 months, when sugar content is reduced to 180-190g/L in ice grape juice Post-fermentation is carried out under the conditions of being transferred to 10 DEG C, carry out 24 hours monitor, the fermentation ends when pol no longer decline, it is cold it is steady qualification after, Ice wine Normal juice is injected in France's dimension card (Vicard) oak barrel in cellar；It is preferred that 225 liters of France's dimension card oak barrels.

To reach optimal mouthfeel, the present invention also uses following methods to ice wine dipper matter, specific steps are as follows:

After the ice wine Normal juice prepared in step (4) is stored sth. in a cellar ageing 9 years in underground, it is divided in oak barrel, 10 I.e. drinkable after storing 1 month under the conditions of DEG C, it can be used repeatedly 2-3 times for oak barrel.

Further, in the step (2) artificial grain it is selected refer to by it is full, hard, not by it is any damage, Solid colour and the grape particle of brownish red, which are chosen, to be come.

Further, the oak barrel in the upgrading step is 2 liters of France's dimension card (Vicard) oak barrels.

The beneficial effects of the present invention are:

(1) what the present invention took is when vineyard nocturnal temperature is lower than -7 DEG C, by the related one section of branch of ice grape fruit ear It cuts, the method being suspended on grape trellis nearby, the collecting method is it is possible to prevente effectively from traditional collecting method causes ice grape to fall Grain is more, and grape branch is easy frostbite, influences the ill effects such as the yield of next year.

(2) in traditional handicraft due in ice grape juice sugar content it is too high, fermentation reaction is difficult to start, thus produce on not only Expensive saccharomycete is needed, and additive amount is 3 times of vin ordinaire or more, causes higher production cost.This hair It is bright to take the mode that saccharomycete activates in advance, so that fermentation reaction is easy starting, but also the usage amount of yeast is made to reduce 90% More than, production cost significantly reduces.

(3) 2 liters of France is used to produce oak barrel to store sth. in a cellar the accurate upgrading of time ice-wine.By multinomial scientific experiment and sense Official judges experiment, proposes that produce oak barrel with 2 liters of France stores 1 month under the conditions of 10 DEG C, stores sth. in a cellar time ice-wine to be promoted Ageing potential quality, and propose oak barrel it can be used repeatedly 2-3 ageing method.The accurate method for upgrading of the ice-wine is simple It is easy, it is scientific and effective.And the faint scent using the ice-wine of the oak barrel upgrading with ice grape intrinsic fragrance and oak, rubber Wooden barrel dress ice-wine is remarkably improved oxidation resistance, and Lipid-soluble antioxidative activity and Water-soluble antioxidant ability compare common ice 2.2 times and 2.0 times are respectively increased in grape wine.Store sth. in a cellar within oak barreled 2010 time ice-wine potassium rich in, receive, calcium, The mineral elements such as iron, zinc, copper, manganese, magnesium, selenium, especially Se content are higher by 300 times than common ice-wine.The present invention has aobvious The social and economic benefit of work.

Detailed description of the invention

Fig. 1 chlorogenic acid standard items full wavelength scanner spectrogram under 190-900nm wavelength condition.

Fig. 2 ice wine difference storage stage Lipid-soluble antioxidative activity and Water-soluble antioxidant ability compare.

Specific embodiment

Further description of the technical solution of the present invention combined with specific embodiments below, but the present invention is not with any shape Formula is limited to embodiment content.Test method described in embodiment is conventional method unless otherwise specified；Such as without special theory Bright, the reagent and biomaterial commercially obtain.

Embodiment 1

1. ice grape harvests: when vineyard nocturnal temperature is lower than -7 DEG C, the related one section of branch of ice grape fruit ear is cut, It is suspended on grape trellis nearby, when nocturnal temperature reaches -10 DEG C--15 DEG C, the fortune in night grape-picking fringe, 2 hours It is carried out to ice Grape processing workshop selected.

2. ice grape is selected and ice-breaking is squeezed the juice: the temperature in selected workshop is -5 DEG C--10 DEG C, and progress artificial grain is selected, Grape particle full, hard, not by any damage, solid colour (brownish red) is chosen, and carries out band immediately Ice-cold squeezing obtains inspissated juice from the crack of frost fruit and filters.Obtain the ice grape that sugar content is up to 410-420g/L Juice.

3. saccharomycete activates: mixing wild grape juice and ice grape juice with the ratio of 2:1 at 20 DEG C, be inoculated with 0.4-0.5g/L Saccharomycete is activated, activation time 48h, and yeast cell number will reach 10 in activating solution⁸A/L.

4. cellar storage: cold fermentation using above-mentioned activating solution as fermentation liquid, is inoculated into ice Portugal in the ratio of 5% (v/v) Main fermentation is carried out in grape juice, fermentation temperature is 15 DEG C, and the main fermentation time is 2-3 months, when sugar content is reduced in ice grape juice Post-fermentation is carried out under the conditions of being transferred to 10 DEG C when 180-190g/L, is carried out 24 hours and is monitored, the fermentation ends when pol is not in decline, It is cold it is steady it is qualified after, inject in the century-old oak barrel of the France in cellar, under micro- oxygen flow state, make that wine is slowly mature, becomes better and approaching perfection day by day, Various minerals, microelement obtain effectively sufficiently concluding, and are like nature itself, the fragrance of a flower, fruity, the sweet fragrant, radix aucklandiae for keeping product special, Graceful fragrance is refreshing.

5. oak barrel upgrading: after above-mentioned ice wine Normal juice stores sth. in a cellar ageing 9 years in underground, in order to further increase the quality of wine, It sets off this and stores sth. in a cellar time ice-wine ageing potential quality, be divided in 2 liters of France and produced in oak barrel, store 1 under the conditions of 10 DEG C It is drunk after a month, it can be used repeatedly 2-3 times for the oak barrel.

Final product quality detection of the present invention

The extraction of 1 ice-wine Content of Chlorogenic Acid and the measurement of content

(1) experimental principle

Volume ratio is used to be extracted for the mixed solution of the ethyl acetate of 1:1 and chloroform, by depressurizing rotary evaporation Purification, ethyl alcohol dissolve extract.The concentration of most suitable extracting solution ethyl alcohol, full wavelength scanner method are determined according to ultraviolet spectrophotometer method Determine the maximum absorption peak of sample.Using the content of high effective liquid chromatography for measuring extract Content of Chlorogenic Acid.

(2) instrument and equipment being related to and reagent are as follows:

(1) instrument and equipment: LC-10A high performance liquid chromatograph；SPD-M10A diode array detector；SIL-10A is automatic Sample injector；LC-10A high pressure pump, Japanese Shimadzu Corporation；HYPERSIL-C18 chromatographic column (5 μm, 250mm, 4.6mm), Dalian Yi Lite scientific instrument Co., Ltd；PL203 type precision electronic balance, Shanghai plum Teller-support benefit Instrument Ltd.；Rotation Evaporimeter, German IKA company；Ultrasound；UV-2600 ultraviolet-uisible spectrophotometer, Japanese Shimadzu Corporation.

(2) reagent: Vidal Blanc (Vidal) ice grape juice, Milan Wu Nvshan, Liaoning Wine Co., Ltd；Chlorogenic acid standard Product；Ethyl alcohol, ethyl acetate, chloroform, phosphate analysis are pure；Acetonitrile chromatographically pure.

(3) determination step

(1) prepared by reference substance solution: precision weighs chlorogenic acid standard items 10mg, is placed in 10mL volumetric flask, adds 50% second Alcohol, dissolution are settled to scale, the chlorogenic acid reference substance stock solution of 1mg/mL are made.Take stock solution 0.2,0.4,0.6,0.8, 1.0mL is added 50% ethyl alcohol and is settled to 5mL, and the control sample solution of 40,80,120,160,200,400 μ g/mL is made.

(2) preparation of test solution: take respectively Vidal Blanc ice-wine former wine and using 1 the method for embodiment into Row oak barrel stores one month, two months, trimestral ice wine 20g, and mixed solution (1 ︰ of 40ml chlorofonn-ethylacetate is added 1) 15min, stratification, are rocked；Upper solution rotary evaporation is taken, until solvent-free steam stopping.Suitable 50% ethyl alcohol is added It washes round-bottomed flask and is settled to 5mL；Mix, through (0.45 μm) of miillpore filter filtering to get.

(3) chromatographic condition

1. measuring the determination of wavelength:

Full wavelength scanner is carried out in 190~900nm using ultraviolet-visible spectrophotometer, chlorogenic acid reference substance exists There is maximum absorption band at 330nm wavelength, see Fig. 1, therefore determines that Detection wavelength is 330nm.

2. measuring chlorogenic acid content:

Chromatographic condition chromatographic column: HYPERSIL-C18 (5 μm, 250mm, 4.6mm)；Mobile phase is that -0.5% phosphoric acid of acetonitrile is molten Liquid 10:90；Flow velocity 1.0mL/min；Column temperature: room temperature；Sample volume: 20 μ L；Detection wavelength 330nm.

(4) result calculates

With peak area (or peak height) for ordinate, standard chlorogenic acid concentration (μ g/mL) is abscissa, and production standard is bent Line.

(5) measurement result of the content of ice-wine Content of Chlorogenic Acid

The content (μ g/g) of 1 ice-wine Content of Chlorogenic Acid of table

(6) conclusion

With the extension of former wine period of storage in oak barrel, chlorogenic acid content is slightly reduced.

2. ice-wine alcoholic strength measures (density bottle method)

(1) principle

With not the waving property substance in way of distillation removal sample, with the density of density bottle method measurement distillate.According to distillate The density of (alcohol water blend), looks into appendix A, the volume fraction of ethyl alcohol, i.e. alcoholic strength when acquiring 20 DEG C, % (volume fraction) table Show.

(2) instrument

Assay balance: sensibility reciprocal 0.0001g；Full glass distiller: 500mL；Water bath with thermostatic control: precision ± 0.1 DEG C；Enclosure temperature meter Density bottle: 25mL or 50mL.

(3) preparation of sample

100mL sample (20 DEG C of liquid temperature) is accurately measured in 500mL cucurbit with a clean, dry 100mL volumetric flask, With 50mL moisture, flush volume bottle, washing lotion are fully incorporated in cucurbit three times, then plus several beades, connect condenser, to take The former volumetric flask of sample makees receiver (additional ice bath).Open cooling water, slow heating distillation.Distillate is collected close to scale, Remove volumetric flask, Gai Sai.30min is kept the temperature in 20.0 DEG C of ± 0.1 DEG C of water-baths, water supplement to scale mixes, spare.

(4) analytical procedure

(1) measurement of water quality is distilled

A) density bottle is cleaned and is dried, band thermometer and side opening cover weigh.It repeats dry and weighs, until constant weight (m).

B) thermometer is removed, the distilled water for being cooled to 15 DEG C or so will be boiled fills the density bottle of constant weight, plug thermometer, There must not be bubble in bottle.Density bottle is immersed in 20.0 DEG C ± 0.1 DEG C of water bath with thermostatic control, to contents temperature up to 20 DEG C, and is protected Hold 10min it is constant after, with filter paper suck side pipe spilling liquid, flush the liquid level in side pipe with side pipe nozzle, cover immediately Side opening cover takes out density bottle, dries the water in bottle wall with filter paper, weighs (m immediately₁)。

(2) measurement of sample mass

Water in density bottle is poured out, with sample (three) repeated flushing density bottle 3 times~5 times, is then filled, by (1) B) same operation, weighs (m₂)。

(5) result calculates

Density of the sample at 20 DEG C is calculated by formula (1), and aerostatic buoyancy corrected value is calculated by formula (2).

In formula:

--- density of the sample at 20 DEG C, unit are gram per liter (g/L)；

The quality of m --- density bottle, unit are gram (g)；

m₁--- the quality of density bottle and water at 20 DEG C, unit are gram (g)；

m₂--- the quality of density bottle and sample at 20 DEG C, unit are gram (g)；

ρ₀--- the density (998.20g/L) of distilled water at 20 DEG C；

A --- aerostatic buoyancy corrected value；

ρ_u--- density value (≈ 1.2g/L) of the dry air in 20 DEG C, 1013.25hPa；

997.0 --- the difference of distilled water and dry air density value at 20 DEG C, unit are gram per liter (g/L).

According to the density of sampleAppendix A is looked into, alcoholic strength is acquired.Acquired results are indicated to a decimal.

(6) precision

The absolute difference of the measurement result independent twice obtained under the conditions of repeatability must not exceed arithmetic mean of instantaneous value 1%.

(7) measurement result of ice wine alcoholic strength

The measurement result of 2 ice wine alcoholic strength of table

3. the total sugar determination of ice-wine (direct titrimetric method)

(1) principle

Using Fehling's solution and reduced sugar azeotropic, the reaction of copper oxidule precipitation is generated, using methylene blue as indicator solution, with Sample or sample after hydrolysis titrate the Fehling's solution boiled, and when reaching terminal, slight excess of reduced sugar is by time of blue Methyl blue be reduced to it is colourless, to show terminal.The content of total reducing sugar or reduced sugar is acquired according to sample consumption.

(2) reagent and material

1, hydrochloric acid solution (1+1)

2, sodium hydroxide solution (200g/L)

3, glucose standards solution (2.5g/L): weigh 105 DEG C~110 DEG C drying in oven 3h and in drier it is cold But DEXTROSE ANHYDROUS 2.5g (being accurate to 0.0001g), is dissolved with water and is settled to 1000mL.

4, Fehling's solution (I, II)

A) it prepares: being prepared by GB/T603

B) it demarcates

Preliminary experiment: Fehling's solution I, II each 5.00mL are drawn in 250mL triangular flask, adds 50mL water, shakes up, in electric furnace On be heated to boiling, titrated under fluidized state with glucose standards solution, when the blue of solution, which disappears, to take on a red color, add 2 drops time Methyl blue indicator solution continues to titrate blue disappearance, records the volume of consumption of glucose standard solution.

Formal test: Fehling's solution I, II each 5.00mL are drawn in 250mL triangular flask, adds 50mL water and compares preliminary experiment The glucose standards solution of few 1mL, is heated to boiling, and keep 2min, adds 2 drop methylene blue indicator solutions, under fluidized state in Terminal is dropped to glucose standards solution in 1min, records the total volume (V) of consumption of glucose standard solution.

C) it calculates

The grams that Fehling's solution I, II each 5mL are equivalent to glucose is calculated by formula (3):

In formula:

F --- Fehling's solution I, II each 5mL are equivalent to the grams of glucose, and unit is gram (g)；

M --- the quality of DEXTROSE ANHYDROUS is weighed, unit is gram (g)；

V --- the total volume of consumption of glucose standard solution, unit are milliliter (mL).

(3) preparation of sample

Accurately draw a certain amount of sample (V₁) [20 DEG C of liquid temperature] in 100mL volumetric flask, being allowed to contained total sugar amount is 0.2g~0.4g adds 5mL hydrochloric acid solution, adds water to 20mL, shakes up.In hydrolyzing 15min in (68 ± 1) DEG C water-bath, take out, it is cold But.It is neutralized to neutrality with sodium hydroxide solution, temperature adjustment adds water to be settled to scale (V to 20 DEG C₂), it is spare.

(4) analytical procedure

Glucose standards solution is replaced with sample, by b) same operation, the volume (V of record consumption sample₃), as a result press formula (4) it calculates.

(5) result calculates

The content of other grape wine total reducing sugars in addition to sack, semi-dry wine is calculated by formula (4).

In formula:

F --- Fehling's solution I, II each 5mL are equivalent to the grams of glucose, and unit is gram (g)；

V₁--- the volume of pipette samples, unit are milliliter (mL)；

V₂--- after sample dilution or the volume of hydrolysis constant volume, unit are milliliter (mL)；

V₃--- the volume of consumption sample, unit are milliliter (mL)；

X --- the content of grape wine total reducing sugar, unit are gram per liter (g/L).

Acquired results are indicated to a decimal.

(6) precision

The absolute difference of the measurement result independent twice obtained under the conditions of repeatability must not exceed arithmetic mean of instantaneous value 2%.

(7) measurement result of ice wine total reducing sugar

The measurement result of 3 ice wine total reducing sugar of table

4. ice-wine sugar-free extract measures

(1) principle

Sample is measured with density bottle method or steams the density of the sample after alcohol, is then looked into appendix C with its density value, is acquired The content of total extractives.Subtract the content of total reducing sugar therefrom again to get the content of sugar-free extract.

(2) instrument

Porcelain evaporating dishes: 200mL；Water bath with thermostatic control: precision ± 0.1 DEG C；Enclosure temperature meter density bottle: 25mL or 50mL.

(3) preparation of sample

100mL sample (20 DEG C of liquid temperature) is measured with 100mL volumetric flask, is poured into 200mL porcelain evaporating dishes, in being evaporated in water-bath One third to about original volume is removed, and after cooling, raffinate carefully moved into former volumetric flask, is repeatedly swung with water and wash evaporation Ware, washing lotion are incorporated in volumetric flask, are settled to scale in 20 DEG C.

The raffinate after steaming alcohol in 2.1 (three) can also be used, be settled to 100mL in 20 DEG C of Shi Yishui.

(4) analytical procedure

Sample is drawn, (four) the same operation by 2.1 in, and density p when calculating 20 DEG C of dealcoholysis sample by 2.1 (five)₁。 With ρ₁× 1.00180 value, looks into appendix C, obtains total extractives content (g/L).

In formula:

ρ₁--- density of the dealcoholysis sample at 20 DEG C, unit are gram per liter (g/L)；

The quality of m --- density bottle, unit are gram (g)；

m₁--- the quality of density bottle and water at 20 DEG C, unit are gram (g)；

m₂--- the quality of density bottle and sample at 20 DEG C, unit are gram (g)；

ρ₀--- the density (998.20g/L) of distilled water at 20 DEG C；

A --- aerostatic buoyancy corrected value；

ρ_u--- density value (≈ 1.2g/L) of the dry air in 20 DEG C, 1013.25hPa；

997.0 --- the difference of distilled water and dry air density value at 20 DEG C, unit are gram per liter (g/L).

--- the correction factor of density bottle volume at 20 DEG C.

According to ρ₁× 1.00180 value, looks into appendix C, acquires total extractives content (g/L).Acquired results are indicated to one Decimal.

(5) precision

The absolute difference of the measurement result independent twice obtained under the conditions of repeatability must not exceed arithmetic mean of instantaneous value 2%.

(6) measurement result of ice wine sugar-free extract

The measurement result of 4 ice wine sugar-free extract of table

5. the total acidity test of ice-wine (indicator method)

(1) principle

It is titrated with phenolphthalein indicator with alkali standard solution using acid base titration principle, total acid is calculated according to the dosage of alkali Content.

(2) reagent and material

Standard Volumetric Solutions for Sodium Hydroxide [c (NaOH)=0.05mol/L]: being prepared and demarcated by GB/T601, and accurate dilute It releases.

Instructions phenolphthalein solution (10g/L): it is prepared by GB/T603.

(3) analytical procedure

(20 DEG C of liquid temperature of pipette samples 2mL；Sampling amount can increase and decrease according to the shade of wine), it is placed in 250mL triangular flask In, 50mL water is added, while 2 drop instructions phenolphthalein solutions are added, after shaking up, is titrated to end with Standard Volumetric Solutions for Sodium Hydroxide immediately Point, and keep non-discolouring in 30s, write down the volume (V of consumption Standard Volumetric Solutions for Sodium Hydroxide₁).Blank test is done simultaneously.

(4) result calculates

The content of total acid is calculated by formula (7) in sample.

In formula:

X --- the content (in terms of tartaric acid) of total acid in sample, unit are gram per liter (g/L)；

The concentration of c --- Standard Volumetric Solutions for Sodium Hydroxide, unit are mole every liter (mol/L)；

V₀--- blank test consumes the volume of Standard Volumetric Solutions for Sodium Hydroxide, and unit is milliliter (mL)；

V₁--- sample drop timing consumes the volume of Standard Volumetric Solutions for Sodium Hydroxide, and unit is milliliter (mL)；

V₂--- the volume of pipette samples, unit are milliliter (mL)；

75 --- the numerical value of the molal weight of tartaric acid, unit are gram every mole (g/moL).

Acquired results are indicated to a decimal.

(5) precision

The absolute difference of the measurement result independent twice obtained under the conditions of repeatability must not exceed arithmetic mean of instantaneous value 5%.

(6) measurement result of ice wine total acid

The measurement result of 5 ice wine total acid of table

The acidity test 6. ice-wine volatilizees

(1) principle

The low boiling point acids i.e. volatile acid in sample is steamed in a manner of distillation, is titrated with alkali standard solution, then survey Determine free sulur dioxide and combine sulfur dioxide, by calculating and correcting, obtains the content of volatile acid in sample.

(2) reagent and solution

Standard Volumetric Solutions for Sodium Hydroxide [c (NaOH)=0.05mol/L]: being prepared and demarcated by GB/T601, and accurate dilute It releases.

Instructions phenolphthalein solution (10g/L): it is prepared by GB/T603.

Hydrochloric acid solution: concentrated hydrochloric acid is diluted with water 4 times.

Iodine standard titration solutionIt prepares and demarcates by GB/T601, and accurate dilutions.

Potassium iodide

Starch indicator solution (5g/L): weighing 5g starch in 500mL water, be heated to boiling, and continues to stir 10min.Again plus Enter 200g sodium chloride, is settled to 1000mL after cooling.

Boratex saturated solution: 5g Boratex (Na is weighed₂B₄O₇·10H₂O it) is dissolved in 100mL hot water, cooling is spare.

(3) analytical procedure

1, it surveys volatile acid: installing distilling apparatus.10mL sample (V) [20 DEG C of liquid temperature] is drawn to be steamed on the apparatus It evaporates, collects 100mL distillate.Distillate is heated to boiling, 2 drop instructions phenolphthalein solutions are added, use Standard Volumetric Solutions for Sodium Hydroxide It is titrated to pink, non-discolouring as terminal in 30s writes down the volume (V of consumption Standard Volumetric Solutions for Sodium Hydroxide₁)。

2, it measures free sulur dioxide: 1 drop hydrochloric acid solution acidification being added in Yu Shangshu solution, 2mL starch indicator solution is added It with several potassium iodide, is titrated after mixing with art iodine standard solution, obtains the volume (V of iodine standard titration solution consumption₂)。

3, measurement combines sulfur dioxide: above-mentioned Boratex saturated solution is added in the above solution, until the aobvious pink of solution, Continue to be titrated with iodine standard titration solution, until solution is blue, obtains the volume (V of iodine standard titration solution consumption₃)。

(4) result calculates

The content that volatile acid is surveyed in sample is calculated by formula (8).

In formula:

X₁--- the content (with Acetometer) of volatile acid is surveyed in sample, unit is gram per liter (g/L)；

The concentration of c --- Standard Volumetric Solutions for Sodium Hydroxide, unit are mole every liter (mol/L)；

V₁--- the volume of consumption Standard Volumetric Solutions for Sodium Hydroxide, unit are milliliter (mL)；

60 --- the numerical value of the molal weight of acetic acid, unit are gram every mole (g/moL)；

The volume of V --- pipette samples, unit are milliliter (mL).

If volatile acid content is near or above physical and chemical index, need to be modified.When amendment, convert by formula (9):

In formula:

X --- true volatile acid (with Acetometer) content in sample, unit are gram per liter (g/L)；

X₁--- actual measurement volatile acid content, unit are gram per liter (g/L)；

c₂--- the concentration of iodine standard titration solution, unit are mole every liter (mol/L)；

The volume of V --- pipette samples, unit are milliliter (mL)；

V₂--- the volume of measurement free sulur dioxide consumption iodine standard titration solution, unit is milliliter (mL)；

V₃--- measurement combines the volume of sulfur dioxide consumption iodine standard titration solution, and unit is milliliter (mL)；

32 --- the numerical value of the molal weight of sulfur dioxide, unit are gram every mole (g/moL)；

1.875 --- 1g free sulur dioxide is equivalent to the quality of acetic acid, and unit is gram (g)；

0.9375 --- 1g combination sulfur dioxide is equivalent to the quality of acetic acid, and unit is gram (g)；

Acquired results are indicated to a decimal.

(5) precision

The absolute difference of the measurement result independent twice obtained under the conditions of repeatability must not exceed arithmetic mean of instantaneous value 5%.

(6) measurement result of ice wine volatile acid

The measurement result of 6 ice wine volatile acid of table

7. free sulur dioxide (oxidizing process)

(1) principle

Under cryogenic, the free sulur dioxide in sample and hydrogen peroxide excessive response generate sulfuric acid, then with alkali mark The sulfuric acid that quasi- solution titration generates.This makes it possible to obtain the contents of free sulur dioxide in sample.

(2) reagent and material

A) it hydrogenperoxide steam generator (0.3%): draws 1mL30% hydrogen peroxide (being stored in refrigerator after unlatching), is diluted with water to 100mL.It is prepared on the day of use.

B) phosphoric acid solution (25%): 295mL85% phosphoric acid is measured, 1000mL is diluted with water to.

C) Standard Volumetric Solutions for Sodium Hydroxide [c (NaOH)=0.01mol/L]: accurate to draw 100mL sodium hydroxide standard Titration solution is settled to 500mL with carbon dioxide-free water.It is stored in the bottle on rubber stopper equipped with soda lime pipe, is reconfigured weekly.

D) it methyl red-methylene blue mixing indicator solution: is prepared by GB/T603.

(3) instrument

A) sulphur dioxide measuring equipment.

B) vacuum pump

(4) analytical procedure

1. sulphur dioxide measuring equipment is connected it is appropriate, I pipe connects with vacuum pump, straight pipe condensation pipe is passed through cooling water.It takes 20mL hydrogenperoxide steam generator is added in pear shape bottle, 5mL peroxidating is added in Drechsel system for lower pear shape bottle and Drechsel system Hydrogen solution, respectively plus after 3 drop mixed indicators, solution immediately becomes purple, instills standard solution of sodium hydroxide, keeps its color lucky Become olive-green, then reinstall it is appropriate, will short neck ball bottle immerse ice bath in.

2. drawing 20.00mL sample (20 DEG C of liquid temperature), from A bottles of addition suitable for reading of C pipe, 10mL phosphoric acid solution is then drawn, Also it is added in short neck ball bottle from snorkel is suitable for reading.

3. opening vacuum pump, makes to be pumped into air mass flow 1000mL/min~1500mL/min, be evacuated 10min.Remove pyriform Bottle, being titrated to reproduction olive-green with Standard Volumetric Solutions for Sodium Hydroxide is terminal, writes down the sodium hydroxide standard drop of consumption Determine the volume number of solution.Sample is replaced to do blank test with water, operation is same as above.Under normal circumstances, solution is not in Drechsel system It should change colour, if solution becomes purple, also need to be measured with Standard Volumetric Solutions for Sodium Hydroxide to olive-green, and will be consumed The volume of Standard Volumetric Solutions for Sodium Hydroxide is added with the volume for the Standard Volumetric Solutions for Sodium Hydroxide that pear shape bottle consumes.

(5) result calculates

The content of free sulur dioxide is calculated by formula (10) in sample.

In formula:

X --- the content of free sulur dioxide in sample, unit are milligrams per liter (mg/L)；

The concentration of c --- Standard Volumetric Solutions for Sodium Hydroxide, unit are mole every liter (mol/L)；

V --- the volume of the Standard Volumetric Solutions for Sodium Hydroxide consumed when measurement sample, unit are milliliter (mL)；

V₀--- the volume of the Standard Volumetric Solutions for Sodium Hydroxide of blank test consumption, unit are milliliter (mL)；

32 --- the numerical value of the molal weight of sulfur dioxide, unit are gram every mole (g/moL)；

20 --- the volume of pipette samples, unit are milliliter (mL)；

Acquired results are indicated to a decimal.

(6) precision

The absolute difference of the measurement result independent twice obtained under the conditions of repeatability must not exceed arithmetic mean of instantaneous value 10%.

(7) measurement result of ice wine free sulur dioxide

The measurement result of 7 ice wine free sulur dioxide of table

8. ice wine and oak metalliferous mineral prime element content

(1) experimental principle

The atom and ion of excitation state are decomposed to form completely using the applied at elevated temperature sample that argon plasma generates, due to swashing Atom and the ion for sending out state are unstable, and outer-shell electron can be from excitation state to low energy level transition, therefore launches the spectral line of feature. After being divided by grating etc., using the intensity of detector detection specific wavelength, the intensity of light is directly proportional to concentration of element to be measured.

(2) instrument and equipment and reagent

(1) instrument and equipment: Leeman labs company, the U.S. Prodigy

(2) reagent: HNO₃Analysis level；H₂O₂Analysis level

(3) determination step

(1) oak powder sample treatment

0.5g oak powder is weighed respectively in counteracting tank, and the dense HNO of 5mL is added₃With the H of 2mL₂O₂, lid is tightened, is placed in micro- 10min is cleared up in wave furnace, after being cooled to room temperature, is transferred in 50mL volumetric flask, with ultrapure water water constant volume, is shaken up to be measured.

(2) ice wine sample treatment

It is each that five female mountain ice wine former wines, oak barrel -1, oak barrel -2, -3 oak barrel -4 of oak barrel, oak barrel -5 are weighed respectively The dense HNO of 10mL is added in 5g, rotary evaporated to dryness₃With the H of 2mL₂O₂, ultrasonic 15min is transferred in the volumetric flask of 100mL, uses Ultrapure water constant volume, it is to be measured.

(3) Instrument operation parameter

Radio-frequency generator power 1100w；Cooling gas flow 20L/min；Atomization air pressure 40psi；Secondary air amount 0.5L/ min；Solution extracted amount 1.5mL/min；Time of integration 15s

(4) result calculates

Each element standard solution and sample solution are measured by Instrument operation parameter, if sample solution concentration is bent beyond standard Sample solution need to be diluted, then be measured by line.Each element content in sample is calculated by following equation (11):

Wherein:

Each element content in X-sample, μ g/g；

The sample solution concentration that C-is checked in by standard curve, μ g/mL；

V-sample solution volume, mL；

N-extension rate；

W-sample mass, g.

(5) ice wine and oak metalliferous mineral prime element assay result

8 five female mountain ice wine of table and oak metalliferous mineral prime element content (μ g/g)

Note: --- expression is not detected

9. the detection of microbiological indicator in ice wine

(1) measuring method

1. microbiological indicator

(1) total number of bacteria: GB 4789.2-2016 national food safety standard food microbiological examination total plate count is surveyed It is fixed

(2) saccharomycete sum: GB 4789.15-2016 national food safety standard food microbiological examination mould and ferment Mother counts

(3) coliform: GB 4789.3-2016 national food safety standard food microbiological examination coliform meter Number

(4) staphylococcus aureus: GB 4789.10-2016 national food safety standard food microbiological examination is golden yellow Color staphylococcus is examined

(5) salmonella: GB 4789.4-2016 national food safety standard food microbiological examination Salmonella bacterial examination It tests

2. the other standards of reference

(1) GB 4789.1-2016 national food safety standard food microbiological examination general provisions.

(2) GB 4789.25-2003 national food safety standard food microbiological examination drinks is examined.

(3) GB 2758-2012 national food safety standard fermented wine and its assembled alcoholic drinks.

(2) measurement result

9 five female mountain ice wine microbial indicators detected result of table

10. five female mountain ice wine are judged

Judge of wine: Hu Wenzhong, Gang be clean, Zou Yu, Jiang Aili, Wang Yanying, Chen Chen, Tian Mixia

10 ice wine of table judges scoring criterion

11. the measurement of ice wine oxidation resistance

(1) experimental principle:

(1) content of the antioxidant in sample is measured using chemoluminescence method.Under ultraviolet light (UV) irradiation, light Quick dose (luminol L) and O₂Reaction generates intermediate product [L^*O₂], the intermediate product again with O₂Interaction generates super oxygen yin Ion radical O₂ ^·-With luminol radical cation.

Its radical reaction formula is as follows:

L+hv(UV)+O₂→[L^*O₂]→L^·++O₂ ^·-

In these free radicals, some is reacted with the polyphenoils in sample, when all polyphenoils are disappeared by free radical After having consumed, remaining Superoxide anions O₂ ^·-Continuation is reacted with luminol radical cation, generates the phthalandione amine yin of excitation state Ion A P^*2-, since the phthalandione amine anion of excitation state is unstable, to return to ground state and shine (blue light), emit light by photoelectricity Multiplier tube detection.It is as follows that it detects reaction formula:

O₂ ^·-+L^·+→N₂+AP^*2-→AP^2-+hv(blue luminescence)

Here, there are two effects for luminol: photosensitizer and detection agent.

(2) luminous signal intensity is continuously detected within the predetermined time by photomultiplier tube.In water-soluble substances In determination oxidative method, free radical is reacted with polyphenoils, a period of time until polyphenoils is depleted Be it is non-luminous, we define this period be lag time (Lag-time).After polyphenoils is depleted, free radical after Continuous reaction, with continuing for reaction, luminous signal intensity is continuously increased, and until maximum value (V), the length of lag time is depended on The content of polyphenoils in sample.In ACW measurement, lag time is defined such that the first derivative calculation by experiment curv Point of inflexion on a curve out, the tangent line of inflection point and the intersection point of X-axis are lag time (Lag-time).There is PCL software in lag time certainly It is dynamic to calculate.

(2) instrument and equipment and reagent

(1) instrument and equipment: Jena, Germany company produces antioxidant and free radical analyzer.

(2) reagent:

Reagent needed for liposoluble substance oxidation resistance is tested

Reagent packet

Reagent name

Reagent 1: methanol

Reagent2: reaction buffer

Reagent 3:PS-1 stock solution (reaction photosensitizer and detection agent), 250 L/ bottles of μ

Reagent4: standard reagent (indicates liposoluble substance to be equivalent to the Trolox (vitamin E) of how many nmol Inoxidizability)

Reagent needed for water-soluble substances oxidation resistance is tested

Reagent packet

Reagent name

Reagent 1: sample solvent

Reagent2: reaction buffer

Reagent 3:PS-1 stock solution (reaction photosensitizer and detection agent), 250 L/ bottles of μ

Reagent4: standard reagent (indicates the anti-oxidant of water-soluble substances to be equivalent to the ascorbic acid of how many nmol Property)

(3) determination step

1. water-soluble substances determination oxidative method

(1) method parameter

As long as lag time can be calculated due to the inflection point for calculating experiment curv, so in measurement process, as long as signal When peaking and beginning to decline, so that it may click " stop " and stop manually.It is not necessary to stop until the ACW method stipulated time Measurement.

(2) blank measure

Cleaning 3 times is first carried out, clicks " Purge → Cleaner 1 ", then measures blank " blank " at least 2 times, it is empty The RSD of white value must not exceed 5%, and until obtaining stationary value, not parallel blank value should be deleted.When blank measure is stablized, System just reaches stable.

(3) canonical measure

5 μ L, 10 μ L, 20 μ L, 30 μ L Reagent4 working solutions (100nmol/L) are pipetted respectively with the liquid-transfering gun of 50 μ L, It is equivalent to the working curve serial solution of 0.5nmol, 1.0nmol, 2.0nmol and 3.0nmol.

When since ascorbic acid is oxidized easily, adding the Reagent4 time as short as possible, while adding Reagent 3 and 4 Between, it mixing time and is inserted into the injection port time and is consistent as far as possible, preferable repeatability available in this way.In addition, surveying every time Before amount, Reagent 1 and Reagent2 is first added, is pre-mixed, then, rapidly joins 4 work of Reagent 3 and Reagent Make solution, after simple mixing, is inserted into injection port measurement.

(4) sample preparation and measurement

It must be aqueous solution or water-soluble substance with the substance that ACW method measures.If the content of sample is more than mark Curve ranges need just to be capable of measuring after being diluted with Reagent 1, guarantee in curve ranges.

2. liposoluble substance determination oxidative method

(1) method parameter

Due to needing to calculate the integrated value of experiment curv, so in a measurement series, blank measure, standard specimen measurement It must be consistent with sample time of measuring.

(2) blank measure

Cleaning 3 times is first carried out, clicks " Purge → Cleaner2+1 ", then measures blank " blank " at least 3 times, it is empty The RSD of white value is preferably no more than 5-10%, and otherwise, blank need to continue to measure, until obtaining stationary value.Not parallel blank value is answered The deletion.When blank measure is stablized, system just reaches stable.

(3) canonical measure

5 μ L, 10 μ L, 20 μ L, 30 μ L Reagent4 working solutions (100nmol/L) are pipetted respectively with the liquid-transfering gun of 50 μ l, It is equivalent to the working curve serial solution of 0.5nmol, 1.0nmol, 2.0nmol and 3.0nmol.Since Torlox is easy by oxygen Change, add the Reagent4 time as short as possible, while adding the time of Reagent 3 and 4, mixing time is use up with the injection port time is inserted into Amount is consistent, preferable repeatability available in this way.In addition, Reagent 1 and Reagent is first added before measurement every time 2, it is pre-mixed, is then quickly added into 4 working solution of Reagent 3 and Reagent, after simple mixing, be inserted into injection port survey Amount.

(4) sample preparation and measurement

The substance of methanol must be dissolved in the substance that acl approach measures.It is of course also apply to that other can be dissolved in organic molten The substance of agent, preferably this organic solvent can dissolve each other with methanol.It is to be noted, however, that: some organic solvents can dissolve Sample cell (plastics), also has certain inoxidizability in this way, causes the measurement result of mistake.So when using other solvents When, a possibility that in order to exclude this error result, secondary control analysis is needed to be implemented (i.e. other than sample, added with solvent Or diluent is into sample).If the content of sample is more than mark curve ranges, need with other of Reagent 1 or selection It is just capable of measuring, guarantees in curve ranges after solvent dilution.If 0.45 μm of organic film mistake need to be used with the presence of particulate matter in sample Filter or centrifugation are removed.

(4) result calculates

1. water-soluble substances oxidation resistance result calculates

Wherein:

Quantity:nmol (in terms of ascorbic acid)

Dilution: extension rate

M: molal weight (ascorbic acid 176.13g/mol)

Pipetted Volume: the volume (μ L) pipetted with liquid-transfering gun

2. liposoluble substance oxidation resistance result calculates

It is calculated using above-mentioned formula (12), (13)

Wherein:

Quantity:nmol (in terms of Trolox)

Dilution: extension rate

M: molal weight (Trolox 250.3g/mol)

Pipetted Volume: the volume (μ l) pipetted with liquid-transfering gun

(5) measurement result:

(1) ice wine and grape wine determination oxidative result

11 ice wine oxidation resistance of table

Result of study shows: compared with former wine, the oxidation resistance for the ice wine being added in oak barrel is significantly increased, oak barrel The Lipid-soluble antioxidative activity and Water-soluble antioxidant ability of the ice wine of middle storage 1 month be respectively 2.197 times of former wine and 2.027 times, but the ice wine stored in oak barrel, oxidation resistance do not increase with the extension of storage time, from storage 1 During a month to 3 months this section, the Lipid-soluble antioxidative activity and Water-soluble antioxidant ability of oak barreled ice wine are protected substantially It holds constant.12. the measurement of polyphenols in ice-wine

(1) principle

Polyphenols in ice-wine is extracted through organic solvent, does mobile phase, high-efficient liquid phase color with methanol and acetic acid Spectrometer RP chromatography is detected, and external standard method is calculated.

(2) instrument and reagent

(1) high performance liquid chromatograph, UV detector

(2) it is cleaned by ultrasonic instrument

(3) Rotary Evaporators

(4) methanol: chromatographically pure；Acetic acid, ethyl acetate, petroleum ether (30-60 DEG C): excellent pure grade

(5) catechin, table catechu, quercetin, coumaric acid, P-hydroxybenzoic acid, caffeic acid, ferulic acid, tannic acid, vanilla Acid, syringic acid standard items: sigma.

(3) chromatographic condition

C₁₈Chromatographic column (4.6mm × 25cm), mobile phase are methanol and acetic acid, flow velocity: 1mL/min, sample volume: 20 μ L, inspection Survey wavelength is 280nm and 320nm.

(4) experimental procedure

(1) standard solution is prepared

A certain amount of polyphenol standard items are weighed respectively, are dissolved with methanol, and the standard solution that concentration is 1mg/mL is made into.Respectively from Table

A certain amount of standard solution is taken out in 1 standard solution in 5mL volumetric flask, with methanol constant volume, is made into different dense Degree

Mixed standard solution, shake up, cross 0.45 μm of film.

The different polyphenol concentration of standard solution of table 12

(2) sample treatment

A) the extraction of ice-wine polyphenol substance

10mL petroleum ether+ethyl acetate (1+ is added in 50mL volumetric flask in the accurate ice-wine sample 10.00mL that measures 1) oscillation extraction 2min, liquid separation are repeated 3 times, and are merged organic phase and are transferred in cucurbit, 40 DEG C of decompression rotary evaporated to dryness, residue It is dissolved in 5.00mL, through 0.45 μm of membrane filtration, for analyzing.

B it) measures

Standard reference material and sample solution are measured by above-mentioned chromatographic condition.

C it) calculates

Each polyphenol component content in ice-wine is calculated by following equation (14):

Wherein:

Each polyphenol content in w-ice-wine, μ g/mL；

The sample solution concentration that c-is checked in by standard curve, μ g/mL；

V₁- sample solution volume, mL；

V₂- volume of sample, mL.

(5) analysis detection result

Each polyphenol content measurement result of 13 ice-wine of table (μ g/mL)

Sample ID	Ice-wine former wine	Oak barrel -1 month	Oak barrel -2 months	Oak barrel -3 months
					Coumaric acid	11.36	16.67	14.27	10.35
Caffeic acid	4.13	4.25	2.96	3.21
					Ferulic acid	1.57	1.52	1.17	1.30
P-hydroxybenzoic acid	2.36	3.70	2.14	1.87
					Tannic acid	192.38	310.72	270.36	317.86
Catechin	8.53	8.16	8.62	9.16
					Vanillic acid	21.20	17.67	17.38	17.52
Quercetin	2.13	1.59	1.51	1.59
					Table catechu	114.82	117.22	104.40	112.46
Syringic acid	16.20	17.05	13.83	16.43

The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it It is interior.

Claims (4)

1. a kind of preparation of ice wine, which comprises the steps of:

(1) ice grape harvests

When vineyard nocturnal temperature is lower than -7 DEG C, the related one section of branch of ice grape fruit ear is cut, is suspended on grape trellis nearby On, when nocturnal temperature reaches -10 DEG C--15 DEG C, in night grape-picking fruit ear, and ice grape is transported within 2 hours and is added Work workshop carries out selected；

(2) ice grape is selected and ice-breaking is squeezed the juice

The temperature in the selected workshop of ice grape is -5 DEG C--10 DEG C, it is selected to carry out artificial grain, and carry out immediately with ice-cold squeezing, from It freezes and obtains inspissated juice in the crack of fruit and filter, obtain the ice grape juice that sugar content is up to 410-420g/L；

(3) saccharomycete activates

Wild grape juice and ice grape juice are mixed with the ratio of 2:1 at 20 DEG C, inoculation 0.4-0.5g/L saccharomycete is activated, living The change time is 48h, and yeast cell number will reach 10 in activating solution⁸A/L.

(4) cold fermentation, cellar storage

Using activating solution obtained by step (3) as fermentation liquid, it is inoculated into ice grape juice in the ratio of 5% (v/v) and carries out main fermentation, Fermentation temperature is 15 DEG C, and the main fermentation time is 2-3 months, is transferred to 10 when sugar content is reduced to 180-190g/L in ice grape juice Post-fermentation is carried out under the conditions of DEG C, carry out 24 hours monitor, the fermentation ends when pol no longer decline, it is cold it is steady qualification after, by ice wine Normal juice is injected in the oak barrel in cellar.

2. referring to satisfy the method according to claim 1, wherein artificial grain is selected in the step (2) Grape particle full, hard, not by any damage, solid colour and brownish red is chosen.

3. a kind of method using oak barrel preservation ice-wine, which is characterized in that ice wine Normal juice is stored sth. in a cellar ageing 9 years in underground Afterwards, it is divided in oak barrel, i.e. drinkable after being stored 1 month under the conditions of 10 DEG C, oak barrel it can be used repeatedly 2-3 It is secondary.

4. according to the method described in claim 2, it is characterized in that, the ice wine is using the method system in claim 1 Standby.