CN103376295A - 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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- CN103376295A CN103376295A CN2013103147963A CN201310314796A CN103376295A CN 103376295 A CN103376295 A CN 103376295A CN 2013103147963 A CN2013103147963 A CN 2013103147963A CN 201310314796 A CN201310314796 A CN 201310314796A CN 103376295 A CN103376295 A CN 103376295A
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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 the grape wine.
Background technology
Grape wine is normally take new fresh grape or grape juice as raw material, and the alcoholic strength that forms through the 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 it is fragrant to be divided into fruital, fermentation perfume (or spice) and ageing according to its source, and wherein ageing perfume (or spice) is from traditional aging process vinous.The tradition Grape Wine Aging is finished in oak barrel, and grape wine can extract multiple oak composition from oak, thereby makes organoleptic quality vinous, comprises that color and luster, transparency, fragrance and convergence etc. are better.But because that oak barrel is made length consuming time, cost height and serviceable life is short etc., so that the use of oak barrel in Grape Wine Aging has certain limitation.In recent years for to satisfy the consumer to the demand of grape wine quality and to reduce the Production of Wine cost, permitted in the world novel Grape Wine Aging method-oak chip ageing.Oak chip mainly comes from the leftover pieces that produce in the 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 before therefore using could improve wine quality through toasting to process.Baking degree can affect the oak chemical composition, such as kind and the content of oak aroma substance, and then affects fragrance vinous.It is low that the oak chip of baking has a cost, and the ageing cycle is short, and do not affect the advantage such as quality vinous,
Both at home and abroad the application in grape wine fragrance is analyzed is more separately about GC-MS and Electronic Nose, as with the impact on oak aroma substance in the grape wine of the baking degree of GC-MS technical research oak; With Electronic Nose Technology different aromas material in the grape wine is distinguished analysis; With Electronic Nose and electronic tongues technology different cultivars grape wine is distinguished.Search is found through patent, 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 be to concentrate on production vinous, brewage the method with ageing, and rarely found about the patent of quick differentiation technology vinous.Usually only use a kind of technology about the research of grape wine fragrance both at home and abroad, use separately Electronic Nose to distinguish fast grape wine, its accuracy remains to be investigated, and use separately the GC-MS technology, it is consuming time longer, can not distinguish fast, seldom have in conjunction with Electronic Nose and the common analysis of two kinds of technology of GC-MS fragrance vinous.With 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 causes a lot of wicked businesses to produce poor quality or low-grade grape wine, adulterates, and has seriously upset Wine Market.Yet there are no report for the vinous quick differentiating method of difference baking degree oak chip in the different ageing time, distinguish fast extremely important to difference baking degree oak chip at the grape wine of different ageing time.
Summary of the invention
The purpose of this invention is to provide oak chip baking degree and the quick differentiating method of ageing time in the grape wine.In order to the impact on grape wine fragrance of consumption, baking degree and ageing vinous time of distinguishing fast and accurately and estimating oak chip; Thereby determine the preferred compositions scheme of several oak chip consumptions, baking degree, ageing time, develop thus the wine product of several different brackets series.
The objective of the invention is to be achieved through the following technical solutions:
The present invention relates to oak chip baking degree and the quick differentiating method of ageing time in a kind of grape wine, comprise the steps:
A, get the grape wine that does not pass through the oak ageing, with its brown port grinding bottle that changes several 500mL over to, guarantee its full bottle;
B, the brown port grinding bottle that will fill wine are divided into several ageing processed group, and the number of ageing processed group is determined that by ageing each ageing processed group contains the brown port grinding bottles of 12 dress wine sample time;
C, slight, the moderate of in the brown port grinding bottle of the dress wine of each ageing processed group, adding respectively 2g, 4g, 6g, 8g and severe baking oak chip, and add sulphurous acid take the concentration of guaranteeing free sulphuric dioxide in the grape wine as 30～40mg/L; Change airtight darkroom over to and carry out ageing;
D, each 50mL of grape wine in the brown port grinding bottle of ageing processed group corresponding to default ageing taking-up sample time;
E, with Electronic Nose the grape wine sample under the permutation and combination of oak chip consumption, oak chip baking degree, ageing asynchronism(-nization) is distinguished analysis; Adopt the GC-MS technology to oak aroma substance quantitative test in the grape wine sample under the described different permutation and combination, and distinguish analysis;
F, analysis result is compared, determine several oak chip consumptions, oak chip baking degree, the assembled scheme of ageing time, develop thus the wine product of several different brackets series.
Above-mentioned grape wine is the Tempranillo from Hispanic 2011 times; Above-mentioned oak chip is U.S. white oak, and slight, moderate and severe baking oak chip in the same size, baking degree have three kinds of slight baking, moderate baking and severe bakings, and the color of oak chip correspondingly from shallow to deep.The ageing processed group is set to be to avoid to cause in the port grinding bottle grape wine not to be in the canful state always and infected or oxidation deterioration by bacterium owing to sampling.
Preferably, in the steps A, the vinous initial physical and chemical index of described not process 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, among the step B, described ageing sample time is 2d, 3d, and 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and 30d (my god); The number of described ageing processed group is 11.Be labeled as respectively ageing 2d, 3d on the brown port grinding bottle of described ageing processed group, 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and 30d; The remaining grape wine of taking a sample in the complete rear port grinding bottle processing of namely cancelling.
Preferably, among the step C, described sulphurous acid is that the volumetric concentration of 150～200 μ L is 6% sulfurous acid solution.
Preferably, among the step C, the condition of described ageing is: steady temperature is room temperature, and constant humidity is 60%～70%.
Preferably, among the step D, the grape wine of taking a sample out need through centrifugal or filtration, be got the supernatant analysis.The reason of processing like this is to avoid the oak chip to disturb.
Preferably, in the 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 rooms clean 360～600s.
Preferably, in the step e, described GC-MS detects need to carry out pre-service to aroma substance in the grape wine sample; Namely use the aroma substance of the concentrated grape wine head space of solid-phase microextraction (solid phase micro-extraction, SPME).The extraction conditions of SPME: get the 8mL fluid sample and be loaded in the 20mL head space bottle, and to wherein adding 2g NaCl, dissolving evenly, add again 0.1mL 3-octanol as interior mark, and the magnetic stir bar of a 10mm specification, use at last rubber cap seal bottle, in 70 ℃ of preheating 5min, then the extracting head (Stableflex Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) of the 50/30 μ m of a Supelco is inserted extraction 40min in liquid level top in the head space bottle.
Preferably, in the step e, described GC-MS testing conditions is: adopt DB-5MS (long 30m, internal diameter 0.25mm, thick coating 0.25 μ m) chromatographic column; Temperature programme: 54 ℃ of initial temperatures, keep 4min, rise to 195 ℃ with 6 ℃/min, rise to 230 ℃ with 2 ℃/min again, keep 10min; The temperature of injection port and detecting device is respectively 230 ℃ and 250 ℃; Carrier gas use purity is 99.999% helium, and without shunt mode, flow velocity is 1.0mL/min.Wherein mass spectral:mass spectrographic testing conditions is: the EI ionization source, electron energy 70eV adopts two kinds of scan pattern-total ion currents (TIC) and selects ion scan (SIM).
Compared with prior art, the present invention has following beneficial effect:
Do not need complicated pre-treatment when 1, Electronic Nose is distinguished grape wine, the detection of distinguishing single grape wine sample only needs 4min, and is fast and convenient; Significantly promote in conjunction with distinguishing accuracy behind the GC-MS.
2, adopt method of the present invention to distinguish fast and accurately different oak chip baking degree, consumption and the grape wine of ageing time; Both can be used for Analysis deterrmination and gone out better oak chip aging process assembled scheme, can be used for again differentiating fast oak chip baking degree similar vinous, consumption and the ageing time of producing.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is that GC-MS is to the quantitative curve of guaiacol.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.Following examples will help those skilled in the art further to understand the present invention, but not limit in any form the present invention.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.
Below the employed grape wine of ageing among each embodiment, satisfy GB to the requirement of the indices of claret.The Electronic Nose that adopts is that the GC-MS device adopts Agilent 7890A GC system and Agilent 5975C MS system available from the iNose of high Shen, Shanghai intelligence Science and Technology Ltd..
Embodiment 1
Grape wine (the Spain that employing is processed without the oak ageing, in 2011 times, Tempranillo), at 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.Its minute installed in the brown port grinding bottle of 132 500mL systems again, and guarantee the full ampuliform attitude of grape wine.Be to guarantee the concentration 30～40mg/L of free sulphuric dioxide in the grape wine, also need in grape wine, to add the sulfurous acid solution of 0.15～0.2mL 6% (v/v).Then will slightly toast, moderate baking and severe baking oak chip (U.S. white oak, slightly, moderate and severe baking oak chip in the same size, along with baking degree by light to weight, the color of oak chip is from shallow to deep) all add respectively different processed group to for 2g, 4g, 6g, 8g by weight, then seal bottle, place the environment (such as airtight darkroom) of lucifuge, sanitation and hygiene, and have steady temperature (room temperature), humidity (65%); The time of total ageing is 30d, at the 2d of ageing, and 3d, 5d, 7d, 9d, 12d, 15d, 18d, 22d, 26d and the 30d 50mL that takes a sample respectively.The grape wine of sampling through centrifugal or filtration, is got the supernatant analysis first; With Electronic Nose Technology the grape wine of the oak chip ageing of difference degree of baking, consumption and the grape wine of ageing different time are done respectively to distinguish research respectively, Electronic Nose gathers fragrance information vinous by sensor.With the GC-MS technology in the grape wine from four kinds of topmost aroma substances of oak: vanillic aldehyde, eugenol, guaiacol (Fig. 1) and syringaldehyde are done quantitative test, and the baking degree of research oak chip and Grape Wine Aging time are on the situation that affects of the content of these four kinds of compositions in the grape wine; As shown in Figure 1, guaiacol concentration is the highest in the grape wine of severe baking oak chip ageing, secondly is moderate baking oak chip, and it is minimum slightly to toast oak chip; When Grape Wine Aging to the in the time of 5 days, the concentration of guaiacol reaches the highest, and ageing is after 9 days, and the concentration of guaiacol tends towards stability.Illustrate before the ageing 9 days, grape wine is very fast to the extraction of aroma substance in the oak chip, and after the ageing 9 days, grape wine is slower to aroma substance extraction rate in the oak chip, simultaneously because the guaiacol structural instability, variously easily be subject to the chemical factors impact and change into other materials, therefore, after the ageing 9 days, the concentration change of guaiacol is less in the grape wine.For same grape wine sample, answer operation repetitive at least 5 times.Analysis result is compared, determine several oak chip consumptions, oak chip baking degree, the assembled scheme of ageing time, develop thus the wine product of several different brackets series.
In the present embodiment, for the sample message that the Electronic Nose sensor gathers, adopt Electronic Nose to carry analysis software: principal component analysis (PCA) PCA and linear discriminant analysis LDA perform an analysis.
Wherein, the 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 rooms clean 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 the 8mL fluid sample and be loaded in the 20mL head space bottle, and to wherein adding 2g NaCl, dissolving evenly, add again 0.1mL 3-octanol as interior mark, and the magnetic stir bar of a 10mm specification, use at last rubber cap seal bottle, in 70 ℃ of preheating 5min, then the extracting head (Stableflex Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) of the 50/30 μ m of a Supelco is inserted extraction 40min in liquid level top in the head space bottle.
GC-MS testing conditions: adopt DB-5MS (long 30m, internal diameter 0.25mm, thick coating 0.25 μ m) chromatographic column.Temperature programme: 54 ℃ of initial temperatures, keep 4min, then rise to 195 ℃ with 6 ℃/min, rise to 230 ℃ with 2 ℃/min again, keep 10min (total run time 58min).The temperature of injection port and detecting device is respectively 230 ℃ and 250 ℃.What carrier gas was used is that purity is 99.999% helium, and without shunt mode, flow velocity is 1.0mL/min.Wherein mass spectral:mass spectrographic testing conditions is: the EI ionization source, electron energy 70eV adopts two kinds of scan pattern-total ion currents (TIC) and selects ion scan (SIM).
More than specific embodiments of the invention are described.It will be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (9)
1. oak chip baking degree and the quick differentiating method of ageing time in the grape wine is characterized in that, comprise the steps:
A, get the grape wine that does not pass through the oak ageing, with its brown port grinding bottle that changes several 500mL over to, guarantee its full bottle;
B, the brown port grinding bottle that will fill wine are divided into several ageing processed group, and the number of ageing processed group is determined that by ageing each ageing processed group contains the brown port grinding bottles of 12 dress wine sample time;
C, slight, the moderate of in the brown port grinding bottle of the dress wine of each ageing processed group, adding respectively 2g, 4g, 6g, 8g and severe baking oak chip, and add sulphurous acid take the concentration of guaranteeing free sulphuric dioxide in the grape wine as 30～40mg/L; Change airtight darkroom over to and carry out ageing;
D, each 50mL of grape wine in the brown port grinding bottle of ageing processed group corresponding to default ageing taking-up sample time;
E, with Electronic Nose the grape wine sample under the permutation and combination of oak chip consumption, oak chip baking degree, ageing asynchronism(-nization) is distinguished analysis; Adopt the GC-MS technology to oak aroma substance quantitative test in the grape wine sample under the described different permutation and combination, and distinguish analysis;
F, analysis result is compared, determine several oak chip consumptions, oak chip baking degree, the assembled scheme of ageing time, develop thus the wine product of several different brackets series.
2. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1, it is characterized in that, in the steps A, the vinous initial physical and chemical index of described not process 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. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1 is characterized in that, among the 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. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1 is characterized in that, among the step C, described sulphurous acid is that the volumetric concentration of 150～200 μ L is 6% sulfurous acid solution.
5. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1 is characterized in that, among the step C, the condition of described ageing is: steady temperature is room temperature, and constant humidity is 60%～70%.
6. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1 is characterized in that, among the step D, the grape wine of taking a sample out need through centrifugal or filtration, be got the supernatant analysis.
7. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1, it is characterized in that, in the step e, described detection by electronic nose condition is: sample gas flow 0.7～1.0L/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 rooms clean 360～600s.
8. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1 is characterized in that, in the step e, described GC-MS detects need to carry out pre-service to aroma substance in the grape wine sample.
9. the quick differentiating method of oak chip baking degree and ageing time in the grape wine as claimed in claim 1 is characterized in that, in the step e, described GC-MS testing conditions is: adopt the DB-5MS chromatographic column; Temperature programme: 54 ℃ of initial temperatures, keep 4min, rise to 195 ℃ with 6 ℃/min, rise to 230 ℃ with 2 ℃/min again, keep 10min; The temperature of injection port and detecting device is respectively 230 ℃ and 250 ℃; Carrier gas use purity is 99.999% helium, and without shunt mode, flow velocity is 1.0mL/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849323A (en) * | 2015-05-06 | 2015-08-19 | 浙江大学 | Method for quickly detecting clarifying agent in 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 |
-
2013
- 2013-07-24 CN CN201310314796.3A patent/CN103376295B/en active Active
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| E.KOUSSISSI等: "Influence of toasting of oak chips on red wine maturation from sensory and gas chromatographic headspace analysis", 《FOOD CHEMISTRY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849323A (en) * | 2015-05-06 | 2015-08-19 | 浙江大学 | Method for quickly detecting clarifying agent in juice based on electronic nose |
| 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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