CN102879496B - Method for researching on bouquet of residue white spirit in wineglass - Google Patents

Method for researching on bouquet of residue white spirit in wineglass Download PDF

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CN102879496B
CN102879496B CN201210369308.4A CN201210369308A CN102879496B CN 102879496 B CN102879496 B CN 102879496B CN 201210369308 A CN201210369308 A CN 201210369308A CN 102879496 B CN102879496 B CN 102879496B
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wineglass
white wine
gas
cup
remains
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CN102879496A (en
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徐占成
王双
徐姿静
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Sichuan Jiannanchun (group) LLC
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Sichuan Jiannanchun (group) LLC
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Abstract

The invention discloses an analysis and detection method, particularly relates to a method for researching on bouquet of residue white spirit in a wineglass and provides a method for researching components of bouquet or residue white spirit in the wineglass. The method includes steps of A, adding white spirit into the wineglass, standing for at least 3 minutes then pouring out the white spirit, and standing the wineglass at the normal temperature for at least one hour; B, collecting bouquet of residue white spirit in the wineglass; C, analyzing the collected bouquet of the white spirit according to a full-two-dimension gas chromatography-flight mass spectrometry, comparing the collected bouquet to a blank sample to determine components of the bouquet of the residue white spirit in the wineglass. By the method, components of the bouquet of the residue white spirit in the wineglass can be analyzed quickly, proportional relation among the components can be determined, and accordingly, data support for researching on residual bouquet of white spirit in empty wineglass is provided.

Description

Research remains in the method for the white wine smell in wineglass
Technical field
The present invention relates to a kind of method of analyzing and testing, especially a kind of research remains in the method for the white wine smell in wineglass.
Background technology
The fragrance of white wine is the first impressions of people to white wine, is a very important factor of judgement white wine quality.Conventionally the description of people's dialogue fume taste has " fragrance is quiet and tastefully laid out, and fragrance is pure, and aftertaste is long, empty cup lasting " etc.The white wine of quality better has preferably the feature of " empty cup lasting " conventionally.A certain amount of white wine is poured in wineglass, then drunk up, although the white wine in wineglass has not had, in cup, still have obvious white wine smell.For high-quality white wine, this smell is very obvious.The white wine that quality is better, its smell remaining in wineglass is more obvious, more allows people feel comfortable, and retention time is also longer.Even empty wineglass is placed to one to two days later, in wineglass, can also smell certain smell.Thus, " empty cup lasting " is also one of characteristic of high-quality white wine, is well received by consumers.Up to this point, also nobody carried out the analysis of system to this white wine smell remaining in wineglass, cannot learn this smell by which kind compound is produced, and the ratio between them how; People can only get on to feel from sense organ the power of this smell.
Summary of the invention
Technical matters to be solved by this invention is to provide the method that research that a kind of detection remains in the white wine odour component in wineglass remains in the white wine smell in wineglass.
The present invention solves the method that research that its technical matters adopts remains in the white wine smell in wineglass, comprises the following steps:
A, in wineglass, add white wine, then after standing at least 3min, outwell white wine, then by wineglass standing at least 1h at normal temperatures; Normal temperature is traditionally arranged to be 10~30 degree.
B, collection remain in the white wine gas in wineglass;
C, utilize comprehensive two dimensional gas chromatography-flight mass spectrum to analyze the white wine gaseous matter of collecting, and contrast with blank sample, thereby determine the constituent that remains in the odoring substance in wineglass.
Be further, described wineglass comprises cup, cup and gas vent, described cup is arranged on the bottom of described cup, described gas vent is arranged on the bottom of cup and connects to described cup inner, on described gas vent, be provided with construction of switch, in A step, described construction of switch is in closed condition; In B step, opening switch structure, utilizes gas vent to collect and remains in the white wine gas in wineglass.
Be further, described wineglass also comprises push rod and piston, and described piston is arranged on push rod end, in B step, utilize push rod to promote piston and be at the uniform velocity pressed into from the opening part of cup, thereby make the white wine gas in cup discharge and collect white wine gas from gas vent.
Further, in B step, thereby white wine gas is passed in ethanol water and dissolves and collect white wine gas; In C step, utilize comprehensive two dimensional gas chromatography-flight mass spectrum to being dissolved with ethanol water and the blank ethanol water of white wine gas, to analyze contrast respectively, thereby determine the constituent that remains in the odoring substance in wineglass.
Further, the ethanol volume ratio of described ethanol water is 55%.
Further, in A step, to adding the amount of white wine in wineglass, be 10ml, after standing 10min, outwell white wine, dry as far as possible the liquid in wineglass, then by wineglass standing 2h at normal temperatures.
The invention has the beneficial effects as follows: the wineglass of this method empty cup lasting after having simulated and having drunk at ordinary times, and the gas of lasting in this wineglass is analyzed, it is easy and simple to handle, and result is accurately and reliably.Use this method to go out the constituent that white wine remains in smell in wineglass than qualitative more quickly, and can determine the proportionate relationship between them, thereby for this phenomenon of researching white spirit " empty cup lasting " provides Data support, break people and can only carry out traditional organoleptic analysis's idea to " empty cup lasting ", this just can improve according to data when making wine, thereby for promoting white wine quality, the white wine of brewageing unique flavor provides strong science support.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of wineglass while containing wine;
Fig. 2 is preferred wineglass schematic diagram;
Fig. 3 is the schematic diagram of collecting while remaining in the white wine gas in wineglass;
Fig. 4 is the analysis result figure of the white wine gas in embodiment;
Fig. 5 is the blank sample analysis result figure in embodiment;
Parts, position and numbering in figure: cup 1, cup 2, gas vent 3, push rod 4, piston 5, receiving flask 6.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
As shown in Figure 1, the present invention includes following steps:
A, in wineglass, add white wine, then after standing at least 3min, outwell white wine, then by wineglass standing at least 1h at normal temperatures; In order to simulate the various situations after drinking, can adopt a plurality of samples, according to containing the time of repose of white wine and the time of repose of empty wineglass, a plurality of samples are set, thereby investigate the white wine gas situation in each situation; After outwelling white wine, should dry as possible, or adopt special drying equipment to carry out normalizing operation;
B, collection remain in the white wine gas in wineglass; Collect white wine gas and can adopt the mode that vacuumizes or push to extract, the gas of collection adopts dissolution with solvents to treat species analysis below; Polar solvent, non-polar solvent or its combination all can be used as solvent, with concrete condition, determine, and by test section material or total material, determine; For example detect Ester and just can adopt ethanol as solvent, if detect whole materials, can adopt ethanol water as solvent;
C, utilize comprehensive two dimensional gas chromatography-flight mass spectrum to analyze the white wine gaseous matter of collecting, and contrast with blank sample, thereby determine the constituent that remains in the odoring substance in wineglass.Blank sample is the solvent of using in simple B step, thereby contrasts, and analyzes material and proportion of composing thereof in white wine gas.
By above-mentioned analytical approach, can adjust wine-making technology according to the material in white wine gas and proportion of composing thereof, thereby obtain the white wine of quality more excellent " empty cup lasting ", this with only rely on and feel to adjust beyond doubt science more.
In order better to collect white wine gas, as shown in Figure 1, described wineglass comprises cup 1, cup 2 and gas vent 3, described cup 2 is arranged on the bottom of described cup 1, described gas vent 3 is arranged on the bottom of cup 1 and connects to described cup 1 inside, on described gas vent 3, be provided with construction of switch, in A step, described construction of switch is in closed condition; In B step, opening switch structure, utilizes gas vent 3 to collect and remains in the white wine gas in wineglass.Wineglass can adopt glass and stupalith to make, and the material of making in view of wineglass is varied, therefore can be made into various wineglasses with various materials, to obtain the most accurate data.Construction of switch, cup 1, cup 2 and gas vent 3 are preferably identical material, to avoid causing interference because material is different when operating.Construction of switch can adopt the pipe close of glass pipe close or other material, the convenient white wine gas that extracts.
In order more thoroughly to collect the white wine gas in wineglass, as shown in Figure 2, described wineglass also comprises push rod 4 and piston 5, described piston 5 is arranged on push rod 4 ends, in B step, utilize push rod 4 to promote piston 5 and be at the uniform velocity pressed into from the opening part of cup 1, thereby make the white wine gas in cup 1 discharge and collect white wine gas from gas vent 3, its process can be participated in shown in Fig. 3.Syringe needle on gas vent 3 goes out to connect, is then inserted into syringe needle in the solvent in receiving flask 6, and when piston 5 is depressed, the white wine gas uniform speed in wineglass is discharged from gas vent 3, thereby is collected the solvent absorption in bottle 6.
Concrete, in B step, thereby white wine gas is passed in ethanol water and dissolves and collect white wine gas; In C step, utilize comprehensive two dimensional gas chromatography-flight mass spectrum to being dissolved with ethanol water and the blank ethanol water of white wine gas, to analyze contrast respectively, thereby determine the constituent that remains in the odoring substance in wineglass.When the white wine gas in same cyath vin detects, adopt two bottles of ethanol waters that proportioning is identical, wherein one bottle absorbs white wine gas, and another bottle contrasts as blank sample.Ethanol water is just in time the good solvent of white wine gas, all substances in its solubilized white wine gas, and the ethanol volume ratio of ethanol water is preferably 55%.By contrast, can analyze material contained in white wine gas and ratio thereof, this has improved good data reference for making wine.
Embodiment
1, key instrument
Full two dimension-flight time gas chromatography mass spectrometry chromatograph; The first chromatographic column DBFFAP of complete two-dimentional gas chromatograph-mass spectrometer; The second chromatographic column DB-1701.Special wineglass, comprises cup 1, push rod 4, piston 5, cup 2 and gas vent 3, and its shape is referring to Fig. 2, and glassware, can be used for collecting white wine and remain in the gas in wineglass.
2, sample and reagent
Certain brand white wine; Top grade straight alcohol, ultrapure water.
3, concrete grammar
(1) in 5 special wineglasses, add respectively 10ml white wine, at normal temperatures and pressures standing 10min; Then outwell white wine, dry with strength wineglass, remove as much as possible liquid wherein, more standing 2h at normal temperatures and pressures.After 2h, in wineglass, without macroscopic liquid, exist, but can also smell stronger white wine wine flavour.Special wineglass cleans with top grade straight alcohol and ultrapure water in advance, and toasts 2h at 150 ℃ of temperature, fully removes residuals wherein.
Special wineglass is straight barrel type water glass, comprises cup 1, push rod 4, piston 5, cup 2 and gas vent 3, and a gas vent 3 is arranged at cup 1 bottom.Cup 1 opening internal diameter is 28.5mm, and integral body is cylindrical shape, and gas vent 3 total lengths are 8mm, and internal diameter is 1.5mm, inside has a grournd glass pipe close as construction of switch, seals.
(2) push rod with Rubber end piston 54 is inserted into gently to the opening of special wineglass, take off the glass pipe close at gas vent 3 places again, next install syringe needle, syringe needle is inserted into gas collection bottle 6 bottoms, in receiving flask 6, contain concentration and be 1 milliliter of 55% ethanol/water solution, referring to Fig. 3.After having connected, slowly and evenly promote push rod 4 downwards, the gas in special wineglass is driven in the ethanol/water solution in gas collection bottle 6 completely.After this process completes, take off gas collection bottle 6, with same procedure by the gas collection in other 4 special wineglasses in this identical gas collection bottle 6.The matched proportion density of ethanol/water solution is the determined optium concentration that can absorb white wine smell after experiment, and ethanol is top grade straight alcohol, the ultrapure water of water treatment.The residual smell of collecting in 5 special wineglasses is in order to increase the concentration in collecting liquid of residual smell, thereby can to them, carry out qualitative analysis more accurately.Syringe needle used and push rod 4 are all first washed through top grade pure wine seminal plasma, then are soaked in ultrapure water, through ultrasonic washing instrument, clean, and then under normal temperature, dry.
Push rod 4 is made for hard plastics processed, has a rubber head piston 5, and rubber head piston 5 diameter 29mm, can combine closely with wineglass opening.Push rod 4 at the uniform velocity downwards, and all gas in wineglass is pushed in gas collection bottle 6.
(3) the good full two dimension-flight time gas chromatography mass spectrometry chromatograph of debugging; Utilize complete two-dimentional gas chromatography mass spectrometry chromatograph to analyze the collection liquid in receiving flask 6, and analysis result and blank collection liquid are before contrasted, can find out at an easy rate the difference between them, thereby complete remaining in the qualitative work of the white wine smell constituent in wineglass.Full two dimension-flight time gas chromatography mass spectrometry chromatograph analysis condition: GC * GC column system: the dual column system that adopts DBFFAP and DB-1701.Injector temperature: 245 ℃; Carrier gas: helium, purity 99.9995%; Constant current, flow: 1.1ml/min; Split ratio: 1:13; ; Modulation period: 4s; Temperature programme condition: first post, column temperature is initiated with 30 ℃, keeps 2min to rise to 80 ℃ with the Cheng Sheng speed of 3 ℃/min, then rises to 255 ℃ with the speed of 5 ℃/min, keeps 32min.Second post, column temperature is initiated with 70 ℃, keeps 2.5min to rise to 85 ℃ with the Cheng Sheng speed of 3 ℃/min, then rises to 260 ℃ with the speed of 5 ℃/min, keeps 32min.Flight mass spectrum frequency acquisition and acquisition range: 50Hz, 30-500u; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 265 ℃.The data obtained enters automatic processing through the workstation of Pegasus 4D again, and qualitative spectrogram used storehouse is NIST/EPA/NIH Version 2.0.The data obtained is again through further processing and draw net result.Result is as Fig. 4 and Fig. 5, and Fig. 4 is the analysis result figure of white wine gas collection liquid, and Fig. 5 is the blank liquid analysis result figure that collects.The blank liquid of collecting is under the same conditions according to identical operation steps gained, just add any wine sample in special wineglass.From Fig. 4 and Fig. 5, can clearly contrast, the blank liquid of collecting of white wine gas collection liquor ratio has obviously had more 6 peaks, and what these 6 peaks represented is exactly the constituent that white wine remains in smell in wineglass.

Claims (5)

1. research remains in the method for the white wine smell in wineglass, it is characterized in that: comprise the following steps: and the wineglass adopting in following steps comprises cup (1), cup (2) and gas vent (3), described cup (2) is arranged on the bottom of described cup (1), described gas vent (3) is arranged on the bottom of cup (1) and connects to described cup (1) inside, and described gas vent is provided with construction of switch on (3);
A, in wineglass, add white wine, and construction of switch is in closed condition, then after standing at least 3min, outwells white wine, then by wineglass standing at least 1h at normal temperatures;
B, opening switch structure, utilize gas vent (3) to collect and remain in the white wine gas in wineglass;
C, utilize comprehensive two dimensional gas chromatography-flight mass spectrum to analyze the white wine gaseous matter of collecting, and contrast with blank sample, thereby determine the constituent that remains in the odoring substance in wineglass.
2. research as claimed in claim 1 remains in the method for the white wine smell in wineglass, it is characterized in that: described wineglass also comprises push rod (4) and piston (5), described piston (5) is arranged on push rod (4) end, in B step, utilize push rod (4) to promote piston (5) and be at the uniform velocity pressed into from the opening part of cup (1), make white wine gas in cup (1) from gas vent (3) thus discharge and collect white wine gas.
3. research as claimed in claim 1 or 2 remains in the method for the white wine smell in wineglass, it is characterized in that: in B step, thereby white wine gas is passed in ethanol water and dissolves and collect white wine gas; In C step, utilize comprehensive two dimensional gas chromatography-flight mass spectrum to being dissolved with ethanol water and the blank ethanol water of white wine gas, to analyze contrast respectively, thereby determine the constituent that remains in the odoring substance in wineglass.
4. research as claimed in claim 3 remains in the method for the white wine smell in wineglass, it is characterized in that: the ethanol volume ratio of described ethanol water is 55%.
5. research as claimed in claim 1 or 2 remains in the method for the white wine smell in wineglass, it is characterized in that: in A step, to adding the amount of white wine in wineglass, be 10ml, after standing 10min, outwell white wine, dry as far as possible the liquid in wineglass, then by wineglass standing 2h at normal temperatures.
CN201210369308.4A 2012-09-28 2012-09-28 Method for researching on bouquet of residue white spirit in wineglass Active CN102879496B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0968518A (en) * 1995-09-01 1997-03-11 Mitsubishi Chem Corp Analyzing method for volatile component of water-soluble polymer
CN101059484A (en) * 2007-04-14 2007-10-24 粟学俐 Use of comprehensive two-dimensional gas chromatography in flavored beer development
CN102636375A (en) * 2012-04-19 2012-08-15 四川剑南春(集团)有限责任公司 Method for extracting target odorant from white wind and white wine odour analysis method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0968518A (en) * 1995-09-01 1997-03-11 Mitsubishi Chem Corp Analyzing method for volatile component of water-soluble polymer
CN101059484A (en) * 2007-04-14 2007-10-24 粟学俐 Use of comprehensive two-dimensional gas chromatography in flavored beer development
CN102636375A (en) * 2012-04-19 2012-08-15 四川剑南春(集团)有限责任公司 Method for extracting target odorant from white wind and white wine odour analysis method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
徐占成等.利用SBSE和全二维气质联用(GC×GC-TOFMS) 新技术解析白酒香味物质的研究.《酿酒科技》.2012,(第7期), *
气相色谱一质谱法测定酒糟、白酒中的芳香族香味成分;赵东等;《酿酒科技》;20061018(第10期);第92-94页 *
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