CN103376295B - Rapid method for distinguishing oak sheet baking degree and ageing time of wine - Google Patents
Rapid method for distinguishing oak sheet baking degree and ageing time of wine Download PDFInfo
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- CN103376295B CN103376295B CN201310314796.3A CN201310314796A CN103376295B CN 103376295 B CN103376295 B CN 103376295B CN 201310314796 A CN201310314796 A CN 201310314796A CN 103376295 B CN103376295 B CN 103376295B
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Abstract
The invention discloses a rapid method for distinguishing oak sheet baking degree and ageing time of wine. The specific method is as below: subpackaging wine without ageing, adding oak sheets and enclosing for ageing; taking wine at preset ageing sampling time; conducting distinguish analysis on wine samples with different permutation and combination of the amount of oak sheets, baking degree and ageing time by using an electronic nose and a GC-MS technology respectively; comparing the analysis results, determining a plurality of combination schemes of the amount of oak sheets, baking degree and ageing time, thereby developing a plurality of wine products of different grades. Distinguishing the wines by the electronic nose employed in the method does not require complex pretreatment, and is rapid and simple; andcombination with the GC-MS distinguish improves the accuracy. Accordingly, the method provided by the invention can be used for accurate analysis and determination of oak sheet ageing technology combination schemes, and can be used for rapid discrimination of baking degree and amount of oak sheets and ageing time of a same kind of wine.
Description
Technical field
The present invention relates to brewing technical field, specifically the quick differentiating method of oak chip baking degree and ageing time in grape wine.
Background technology
Grape wine normally with new fresh grape or grape juice for raw material, the alcoholic strength through culture propagation brew is not less than the general name of all kinds of wine of 7% (v/v).Fragrance is important quality vinous, and can be divided into fruital according to its source, fermentation is fragrant and ageing is fragrant, wherein ageing is fragrant from traditional aging process vinous.Traditional wine ageing completes in oak barrel, and grape wine can extract multiple oak composition from oak, thus makes organoleptic quality vinous, comprises color and luster, transparency, fragrance and convergence etc. better.But due to oak barrel, to make length consuming time, cost high and serviceable life short etc., makes the use of oak barrel in Grape Wine Aging have a definite limitation.In recent years reducing Production of Wine cost for meeting consumer to the demand of grape wine quality, have granted novel Grape Wine Aging method-oak chip ageing in the world.Oak chip mainly comes from the leftover pieces produced in oak barrel manufacturing process, and moisture is up to about 70%, and the content of bitter taste tannin is high especially, and aroma substance is few, needs could improve wine quality through baking process before therefore using.Baking degree can affect oak chemical composition, as kind and the content of oak aroma substance, and then affects fragrance vinous.It is low that the oak chip toasted has cost, and the ageing cycle is short, and does not affect the advantages such as quality vinous,
Both at home and abroad about GC-MS and the application of Electronic Nose separately in Wine Aroma is analyzed more, as with the baking degree of GC-MS technical research oak on the impact of oak aroma substance in grape wine; Carry out differentiation by Electronic Nose Technology to different aromas material in grape wine to analyze; By Electronic Nose and electronic tongues technology, different cultivars grape wine is distinguished.Find through patent search, application number: 201210175444.X, a kind of air-dry claret brewage process by name; Application number: 201210175442.0, a kind of mummification ageing method vinous by name; Application number: 201210005121.6, a kind of ageing type producing process for dry red wine by name, mostly these technology are to concentrate on production vinous, brewage the method with ageing, and rarely found about the patent distinguishing technology vinous fast.Usually a kind of technology is only used both at home and abroad about the research of Wine Aroma, be used alone Electronic Nose and distinguish grape wine fast, its accuracy needs to be investigated, and be used alone GC-MS technology, it is consuming time longer, can not distinguish fast, seldom have and jointly analyze fragrance vinous in conjunction with Electronic Nose and GC-MS two kinds of technology.By Electronic Nose Technology and the coupling of GC-MS technology, can, in conjunction with two kinds of technology advantage separately, make precision of analysis high, easy, quick.
Grape wine consumption market expanding day and lucrative, cause a lot of wicked business to produce poor quality or low-grade grape wine, adulterate, very disruptive Wine Market.Difference baking degree oak chip be have not been reported at the vinous quick differentiating method of different ageing time, distinguish extremely important to difference baking degree oak chip fast at the grape wine of different ageing time.
Summary of the invention
The object of this invention is to provide the quick differentiating method of oak chip baking degree and ageing time in grape wine.In order to distinguish and to evaluate the consumption of oak chip, baking degree and ageing time vinous fast and accurately to the impact of Wine Aroma; Thus determine the preferred compositions scheme of several oak chip consumption, baking degree, ageing time, develop the wine product of several different brackets series thus.
The object of the invention is to be achieved through the following technical solutions:
The present invention relates to the quick differentiating method of oak chip baking degree and ageing time in a kind of grape wine, comprise the steps:
A, get grape wine without oak ageing, proceeded to the brown port grinding bottle of several 500mL, ensure its full bottle;
B, by dress wine brown port grinding bottle be divided into several ageing processed group, the number of ageing processed group is determined by ageing sample time, each ageing processed group containing 12 dress wine brown port grinding bottle;
C, slight, the moderate of adding 2g, 4g, 6g, 8g in the brown port grinding bottle of the dress wine of each ageing processed group respectively and heavy toast oak chip, and add sulphurous acid to guarantee that the concentration of free sulur dioxide in grape wine is for 30 ~ 40mg/L; Proceed to airtight darkroom and carry out ageing;
D, each 50mL of grape wine taken out in ageing sample time of presetting in the brown port grinding bottle of corresponding ageing processed group;
E, by Electronic Nose, differentiation is carried out to the wine samples under oak chip consumption, oak chip baking degree, ageing time different permutation and combination and analyze; Adopt GC-MS technology to oak aroma substance quantitative test in the wine samples under described different permutation and combination, and carry out differentiation analysis;
F, analysis result to be compared, determine several oak chip consumption, oak chip baking degree, the assembled scheme of ageing time, develop the wine product of several different brackets series thus.
Above-mentioned grape wine is the Tempranillo from Hispanic 2011 times; Above-mentioned oak chip is U.S. white oak, slight, moderate and heavy toast oak chip in the same size, baking degree has slight baking, moderate baking and heavy toast three kinds, and the color of oak chip is correspondingly from shallow to deep.Arrange ageing processed group to be to avoid causing grape wine in port grinding bottle not to be in canful state always and to be infected by bacterial or oxidation deterioration due to sampling.
Preferably, in steps A, the described vinous initial physical and chemical index without oak ageing is: volatile acid 0.79g/L, total acid 5.4g/L, total reducing sugar 3.9g/L, sugar-free extract 20.9g/L, alcoholic strength 11.65 (v/v), pH 3.54, free sulur dioxide 15.98mg/L, total sulfur dioxide 79.92mg/L.
Preferably, in step B, described ageing be sample time 2d, 3d, 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and 30d (my god); The number of described ageing processed group is 11.The brown port grinding bottle of described ageing processed group is labeled as ageing 2d, 3d, 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and 30d respectively; After sampling, in port grinding bottle, namely remaining grape wine cancel process.
Preferably, in step C, described sulphurous acid is the volumetric concentration of 150 ~ 200 μ L is the sulfurous acid solution of 6%.
Preferably, in step C, the condition of described ageing is: steady temperature is room temperature, and constant humidity is 60% ~ 70%.
Preferably, in step D, the grape wine sampled out through centrifugal or filtration, need get supernatant analysis.The reason of such process is to avoid oak chip to disturb.
Preferably, in step e, described detection by electronic nose condition is: sample gas flow 0.7 ~ 1.0 L/min, detection time, 240 ~ 300s, waited for sample injection time 10 ~ 20s, each sample do 5 times parallel, scavenging period 60 ~ 300s between parallel sample, different sample room cleaning 360 ~ 600s.
Preferably, in step e, described GC-MS detects to be needed to carry out pre-service to aroma substance in wine samples; Namely the aroma substance of the concentrated grape wine head space of solid-phase microextraction (solid phase micro-extraction, SPME) is used.The extraction conditions of SPME: get 8mL fluid sample and be loaded in 20mL ml headspace bottle, and add 2g NaCl wherein, be uniformly dissolved, add 0.1mL 3-octanol again as interior mark, and the magnetic stir bar of a 10mm specification, finally use rubber cap seal bottle, in 70 DEG C of preheating 5min, then the extracting head (Stableflex Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) of 50/30 of a Supelco μm is inserted ullage extraction 40min in ml headspace bottle.
Preferably, in step e, described GC-MS testing conditions is: adopt DB-5MS (long 30m, internal diameter 0.25mm, thick coating 0.25 μm) chromatographic column; Temperature programme: initial temperature 54 DEG C, keeps 4min, rises to 195 DEG C, then rise to 230 DEG C with 2 DEG C/min with 6 DEG C/min, keeps 10min; The temperature of injection port and detecting device is 230 DEG C and 250 DEG C respectively; Carrier gas uses purity to be the helium of 99.999%, and without shunt mode, flow velocity is 1.0mL/min.Wherein mass spectrographic testing conditions is: EI ionization source, electron energy 70eV, adopts two kinds of scan pattern-total ion currents (TIC) and Selective ion mode scanning (SIM).
Compared with prior art, the present invention has following beneficial effect:
1, do not need complicated pre-treatment when Electronic Nose distinguishes grape wine, the detection distinguishing single wine samples only needs 4min, fast and convenient; Significantly promote in conjunction with distinguishing accuracy after GC-MS.
2, method of the present invention is adopted can to distinguish fast and accurately different oak chip baking degree, consumption and the grape wine of ageing time; Both can be used for analysis and determined preferably oak chip aging process assembled scheme, the oak chip baking degree similar vinous that can be used for again differentiating fast to produce, consumption and ageing time.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the quantitation curves of GC-MS to guaiacol.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make certain adjustments and improvements.These all belong to protection scope of the present invention.
The grape wine that in following embodiment, ageing uses, meets the requirement of GB to the indices of claret.The Electronic Nose adopted holds high the iNose of Shen intelligence Science and Technology Ltd., and GC-MS device adopts Agilent 7890A GC system and Agilent 5975C MS system.
embodiment 1
Adopt the grape wine (Spain without oak ageing process, 2011 times, Tempranillo), first measure initial physical and chemical index vinous, its initial physical and chemical index is: volatile acid 0.79g/L, total acid 5.4g/L, total reducing sugar 3.9g/L, sugar-free extract 20.9g/L, alcoholic strength 11.65 (v/v), pH 3.54, free sulur dioxide 15.98mg/L, total sulfur dioxide 79.92mg/L.Be dispensed into again in the brown port grinding bottle of 132 500mL, and ensured the full ampuliform state of grape wine.For ensureing the concentration 30 ~ 40mg/L of free sulur dioxide in grape wine, also need the sulfurous acid solution of 6% (v/v) adding 0.15 ~ 0.2mL in grape wine.Then will slightly toast, moderate baking and heavy toast oak chip (U.S. white oak, slightly, moderate and heavy toast oak chip in the same size, along with baking degree from light to heavy, the color of oak chip is from shallow to deep) all add different processed group respectively to for 2g, 4g, 6g, 8g by weight, then bottle is sealed, be placed in the environment (as airtight darkroom) of lucifuge, sanitation and hygiene, and there is steady temperature (room temperature), humidity (65%); The time of total ageing is 30d, and at the 2d of ageing, 3d, 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and 30d sample 50mL respectively.The grape wine of sampling, first through centrifugal or filtration, gets supernatant analysis; Do respectively to distinguish research to the grape wine of the oak chip ageing of difference degree of baking, consumption and the grape wine of ageing different time by Electronic Nose Technology respectively, Electronic Nose gathers fragrance information vinous by sensor.With GC-MS technology in grape wine from four of oak kinds of topmost aroma substances: vanillic aldehyde, eugenol, guaiacol (Fig. 1) and syringaldehyde do quantitative test, and the research baking degree of oak chip and Grape Wine Aging time affect situation to the content of these four kinds of compositions in grape wine; As shown in Figure 1, in the grape wine of heavy toast oak chip ageing, guaiacol concentration is the highest, and be secondly moderate baking oak chip, slight baking oak chip is minimum; When Grape Wine Aging was by the 5th day, the concentration of guaiacol reaches the highest, and ageing is after 9 days, and the concentration of guaiacol tends towards stability.Before ageing 9 days is described, grape wine is very fast to the extraction of aroma substance in oak chip, and after ageing 9 days, grape wine is slower to aroma substance extraction rate in oak chip, simultaneously due to guaiacol structural instability, be easily variously subject to chemical factors impact and change into other materials, therefore, ageing is after 9 days, and in grape wine, the concentration change of guaiacol is less.For same wine samples, answer operation repetitive at least 5 times.Analysis result is compared, determines several oak chip consumption, oak chip baking degree, the assembled scheme of ageing time, develop the wine product of several different brackets series thus.
In the present embodiment, for the sample message that Electronic Nose sensor gathers, Electronic Nose is adopted to carry analysis software: principal component analysis (PCA) PCA and linear discriminant analysis LDA performs an analysis.
Wherein, detection by electronic nose condition is: sample gas flow 0.7 ~ 1.0L/min, and detection time, 240 ~ 300s, waited for sample injection time 10 ~ 20s, scavenging period 60 ~ 300s between parallel sample, different sample room cleaning 360 ~ 600s.
In the present embodiment, GC-MS detects needs pre-treatment, namely concentrates the aroma substance of grape wine head space with solid-phase microextraction SPME.
Wherein, the extraction conditions of SPME: get 8mL fluid sample and be loaded in 20mL ml headspace bottle, and add 2g NaCl wherein, be uniformly dissolved, add 0.1mL 3-octanol again as interior mark, and the magnetic stir bar of a 10mm specification, finally use rubber cap seal bottle, in 70 DEG C of preheating 5min, then the extracting head (Stableflex Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) of 50/30 of a Supelco μm is inserted ullage extraction 40min in ml headspace bottle.
GC-MS testing conditions: adopt DB-5MS (long 30m, internal diameter 0.25mm, thick coating 0.25 μm) chromatographic column.Temperature programme: initial temperature 54 DEG C, keeps 4min, then rises to 195 DEG C with 6 DEG C/min, then rise to 230 DEG C with 2 DEG C/min, keeps 10min (total run time 58min).The temperature of injection port and detecting device is 230 DEG C and 250 DEG C respectively.Carrier gas use purity be 99.999% helium, without shunt mode, flow velocity is 1.0mL/min.Wherein mass spectrographic testing conditions is: EI ionization source, electron energy 70eV, adopts two kinds of scan pattern-total ion currents (TIC) and Selective ion mode scanning (SIM).
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (6)
1. the quick differentiating method of oak chip baking degree and ageing time in grape wine, is characterized in that, comprise the steps:
A, get grape wine without oak ageing, proceeded to the brown port grinding bottle of several 500mL, ensure its full bottle;
B, by dress wine brown port grinding bottle be divided into several ageing processed group, the number of ageing processed group is determined by ageing sample time, each ageing processed group containing 12 dress wine brown port grinding bottle;
C, slight, the moderate of adding 2g, 4g, 6g, 8g in the brown port grinding bottle of the dress wine of each ageing processed group respectively and heavy toast oak chip, and add sulphurous acid to guarantee that the concentration of free sulur dioxide in grape wine is for 30 ~ 40mg/L; Proceed to airtight darkroom and carry out ageing;
D, each 50mL of grape wine taken out in ageing sample time of presetting in the brown port grinding bottle of corresponding ageing processed group;
E, by Electronic Nose, differentiation is carried out to the wine samples under oak chip consumption, oak chip baking degree, ageing time different permutation and combination and analyze; Adopt GC-MS technology to oak aroma substance quantitative test in the wine samples under described different permutation and combination, and carry out differentiation analysis; Described oak aroma substance is vanillic aldehyde, eugenol, guaiacol and syringaldehyde;
F, analysis result to be compared, determine several oak chip consumption, oak chip baking degree, the assembled scheme of ageing time, develop the wine product of several different brackets series thus;
In step e, described detection by electronic nose condition is: sample gas flow 0.7 ~ 1.0L/min, detection time 240 ~ 300s, wait for sample injection time 10 ~ 20s, each sample do 5 times parallel, scavenging period 60 ~ 300s between parallel sample, different sample room cleaning 360 ~ 600s;
Described GC-MS detects to be needed to carry out pre-service to aroma substance in wine samples; Described pre-service is the aroma substance concentrating grape wine head space with solid-phase microextraction SPME;
Described GC-MS testing conditions is: adopt DB-5MS chromatographic column; Temperature programme: initial temperature 54 DEG C, keeps 4min, rises to 195 DEG C, then rise to 230 DEG C with 2 DEG C/min with 6 DEG C/min, keeps 10min; The temperature of injection port and detecting device is 230 DEG C and 250 DEG C respectively; Carrier gas uses purity to be the helium of 99.999%, and without shunt mode, flow velocity is 1.0mL/min.
2. oak chip baking degree and the quick differentiating method of ageing time in grape wine as claimed in claim 1, it is characterized in that, in steps A, the described vinous initial physical and chemical index without oak ageing is: volatile acid 0.79g/L, total acid 5.4g/L, total reducing sugar 3.9g/L, sugar-free extract 20.9g/L, alcoholic strength 11.65v/v, pH 3.54, free sulur dioxide 15.98mg/L, total sulfur dioxide 79.92mg/L.
3. oak chip baking degree and the quick differentiating method of ageing time in grape wine as claimed in claim 1, is characterized in that, in step B, described ageing sample time is 2d, 3d, 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and 30d; The number of described ageing processed group is 11.
4. oak chip baking degree and the quick differentiating method of ageing time in grape wine as claimed in claim 1, it is characterized in that, in step C, described sulphurous acid is the volumetric concentration of 150 ~ 200 μ L is the sulfurous acid solution of 6%.
5. oak chip baking degree and the quick differentiating method of ageing time in grape wine as claimed in claim 1, it is characterized in that, in step C, the condition of described ageing is: steady temperature is room temperature, and constant humidity is 60% ~ 70%.
6. oak chip baking degree and the quick differentiating method of ageing time in grape wine as claimed in claim 1, is characterized in that, in step D, the grape wine sampled out through centrifugal or filtration, need get supernatant analysis.
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| CN104849323B (en) * | 2015-05-06 | 2017-06-30 | 浙江大学 | A kind of method of fining agent in quick detection fruit juice based on Electronic Nose |
| CN105606420A (en) * | 2016-01-08 | 2016-05-25 | 华南理工大学 | Method for rapidly and accurately measuring content of total acid in food based on phase conversion reaction |
| CN106190683A (en) * | 2016-09-07 | 2016-12-07 | 西京学院 | A kind of combined type health care preparation of wine |
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