CN102879496A - 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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Publication number
CN102879496A
CN102879496A CN2012103693084A CN201210369308A CN102879496A CN 102879496 A CN102879496 A CN 102879496A CN 2012103693084 A CN2012103693084 A CN 2012103693084A CN 201210369308 A CN201210369308 A CN 201210369308A CN 102879496 A CN102879496 A CN 102879496A
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wineglass
liquor
gas
cup
remains
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CN102879496B (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 liquor smell in the 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 liquor smell in the wineglass.
Background technology
The fragrance of liquor be people to the first impression of liquor, be a very important factor judging the liquor quality.Usually the description of people's dialogue fume flavor has " fragrance is quiet and tastefully laid out, and fragrance is pure, and aftertaste is long, empty cup lasting " etc.The liquor of quality better has preferably the characteristics of " empty cup lasting " usually.A certain amount of liquor is poured in the wineglass, then drunk up, although the liquor in the wineglass has not had, in the cup apparent in view liquor smell is arranged still.For high-quality liquor, this smell is very obvious.The liquor that quality is better, its smell that remains in the wineglass is more obvious, more allows the people feel comfortable, and retention time is also longer.Even empty wineglass placed one to two days later, can also smell certain smell in the wineglass.Thus, " empty cup lasting " also is one of characteristic of high-quality liquor, is well received by consumers.Up to this point, also nobody carried out the analysis of system to this liquor smell that remains in the wineglass, can't 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 provides the method that research that a kind of detection remains in the liquor odour component in the wineglass remains in the liquor smell in the wineglass.
The present invention solves the method that research that its technical matters adopts remains in the liquor smell in the wineglass, may further comprise the steps:
A, in wineglass, add liquor, then leave standstill at least and outwell liquor behind the 3min, then wineglass is left standstill at least 1h at normal temperatures; Normal temperature is traditionally arranged to be 10~30 degree.
B, collection remain in the liquor gas in the wineglass;
C, utilize comprehensive two dimensional gas chromatography-flight mass spectrum that the liquor gaseous matter of collecting is analyzed, and compare with blank sample, thereby determine the constituent that remains in the odoring substance in the wineglass.
Further be, 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, be provided with construction of switch on the described gas vent, in the A step, described construction of switch is in closed condition; In the B step, the opening switch structure utilizes gas vent to collect the liquor gas that remains in the wineglass.
Further be, described wineglass also comprises push rod and piston, and described piston is arranged on the push rod end, in the B step, utilize the push rod pushing piston at the uniform velocity to be pressed into from the opening part of cup, thereby collect liquor gas so that the liquor gas in the cup is discharged from gas vent.
Further be in the B step, thereby liquor gas to be passed into dissolving collection liquor gas in the ethanol water; In the C step, utilize comprehensive two dimensional gas chromatography-flight mass spectrum respectively the ethanol water and the blank ethanol water that are dissolved with liquor gas to be analyzed contrast, thereby determine the constituent that remains in the odoring substance in the wineglass.
Further be that the ethanol volume ratio of described ethanol water is 55%.
Further be, in the A step, the amount that adds liquor in the wineglass is 10ml, outwells liquor after leaving standstill 10min, dries as far as possible the liquid in the wineglass, then wineglass is left standstill 2h at normal temperatures.
The invention has the beneficial effects as follows: this method has been simulated the wineglass of the rear empty cup lasting of drinking at ordinary times, and the gas of lasting in this wineglass is analyzed, and it is easy and simple to handle, and the result accurately and reliably.Use this method to go out the constituent that liquor remains in smell in the 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, broken people can only carry out traditional organoleptic analysis to " empty cup lasting " idea, this just can improve when making wine according to data, thereby for promoting the liquor quality, the liquor of brewageing unique flavor provides strong science support.
Description of drawings
Fig. 1 is the synoptic diagram of wineglass when containing wine;
Fig. 2 is preferred wineglass synoptic diagram;
Fig. 3 is the synoptic diagram when collecting the liquor gas that remains in the wineglass;
Fig. 4 is the analysis result figure of the liquor gas among the embodiment;
Fig. 5 is the blank sample analysis result figure among the embodiment;
Parts, position and numbering among the figure: cup 1, cup 2, gas vent 3, push rod 4, piston 5, receiving flask 6.
Embodiment
The invention will be further described below in conjunction with accompanying drawing.
As shown in Figure 1, the present invention includes following steps:
A, in wineglass, add liquor, then leave standstill at least and outwell liquor behind the 3min, then wineglass is left standstill at least 1h at normal temperatures; In order to simulate the various situations after drinking, can adopt a plurality of samples, namely according to the time of repose of containing liquor and the time of repose of empty wineglass a plurality of samples are set, thereby investigate the liquor gas situation in each situation; After outwelling liquor, should dry as possible, perhaps adopt special drying equipment to carry out normalizing operation;
B, collection remain in the liquor gas in the wineglass; Collect liquor gas and can adopt the mode that vacuumizes or push to extract, the gas of collection adopts dissolution with solvents to treat the species analysis of back; Polar solvent, non-polar solvent or its combination all can be used as solvent, decide with concrete condition, namely determine by test section material or total material; For example detect Ester and just can adopt ethanol as solvent, then can adopt ethanol water as solvent if detect whole materials;
C, utilize comprehensive two dimensional gas chromatography-flight mass spectrum that the liquor gaseous matter of collecting is analyzed, and compare with blank sample, thereby determine the constituent that remains in the odoring substance in the wineglass.Blank sample is the solvent of using in the simple B step, thereby compares, and analyzes material and proportion of composing thereof in the liquor gas.
By above-mentioned analytical approach, can adjust wine-making technology according to the material in the liquor gas and proportion of composing thereof, thereby obtain the liquor of quality more excellent " empty cup lasting ", this feels to adjust beyond doubt more science with only relying on.
In order better to collect liquor 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, be provided with construction of switch on the described gas vent 3, in the A step, described construction of switch is in closed condition; In the B step, the opening switch structure utilizes gas vent 3 to collect the liquor gas that remains in the 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 of the material difference when operating.Construction of switch can adopt the pipe close of glass pipe close or other material, the convenient liquor gas that extracts.
In order more thoroughly to collect the liquor gas in the 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 the B step, utilize push rod 4 pushing pistons 5 at the uniform velocity to be pressed into from the opening part of cup 1, thereby collect liquor gas so that the liquor gas in the cup 1 is discharged from gas vent 3, its process can be participated in shown in Figure 3.Then syringe needle on gas vent 3 goes out to connect is inserted into syringe needle in the solvent in the receiving flask 6, and when piston 5 was depressed, the liquor gas uniform speed in the wineglass was discharged from gas vent 3, thereby is collected the solvent absorption in the bottle 6.
Concrete, in the B step, thereby liquor gas is passed into dissolving collection liquor gas in the ethanol water; In the C step, utilize comprehensive two dimensional gas chromatography-flight mass spectrum respectively the ethanol water and the blank ethanol water that are dissolved with liquor gas to be analyzed contrast, thereby determine the constituent that remains in the odoring substance in the wineglass.When detecting with the liquor gas in the cyath vin, adopt two bottles of ethanol waters that proportioning is identical, wherein one bottle absorbs liquor gas, and another bottle compares as blank sample.Ethanol water just in time is the good solvent of liquor gas, all substances in its solubilized liquor gas, and the ethanol volume ratio of ethanol water is preferably 55%.Can analyze material contained in the liquor gas and ratio thereof by contrast, this has improved good data reference for wine brewing.
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 liquor and remains in gas in the wineglass.
2, sample and reagent
Certain brand liquor; The top grade straight alcohol, ultrapure water.
3, concrete grammar
(1) in 5 special wineglasses, adds respectively 10ml liquor, leave standstill at normal temperatures and pressures 10min; Then outwell liquor, dry with strength wineglass, remove as much as possible liquid wherein, leave standstill at normal temperatures and pressures again 2h.Exist without macroscopic liquid in the wineglass behind the 2h, but can also smell stronger liquor wine flavour.Special wineglass cleans with top grade straight alcohol and ultrapure water in advance, and toasts 2h under 150 ℃ of temperature, fully removes residuals wherein.
Special wineglass is the 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, in a grournd glass pipe close is arranged as construction of switch, seal.
(2) will be inserted into gently with the push rod 4 of Rubber end piston 5 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, contain concentration in the receiving flask 6 and be 1 milliliter of 55% ethanol/water solution, referring to Fig. 3.Connect finish after, slowly and evenly promote push rod 4 downwards, the gas in the special wineglass is driven in the ethanol/water solution in the gas collection bottle 6 fully.After this process is finished, take off gas collection bottle 6, with same procedure with 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 the liquor smell after experiment, and ethanol is the top grade straight alcohol, the ultrapure water of water treatment.Collect residual smell in 5 special wineglasses and be in order to increase the concentration in collecting liquid of residual smell, thereby can carry out qualitative analysis to them more accurately.Used syringe needle and push rod 4 all pass through first top grade alcohol alcohol wash, are soaked in the ultrapure water again, clean through ultrasonic washing instrument, then dry under the normal temperature.
Push rod 4 is made for hard plastics processed, and a rubber head piston 5 is arranged, and rubber head piston 5 diameter 29mm can combine closely with the wineglass opening.Push rod 4 at the uniform velocity downwards, and all gas in the wineglass is pushed in the gas collection bottle 6.
(3) the good full two dimension of debugging-flight time gas chromatography mass spectrometry chromatograph; Utilize complete two-dimentional gas chromatography mass spectrometry chromatograph that the collection liquid in the receiving flask 6 is analyzed, and analysis result and before blank are collected liquid compare, can find out at an easy rate the difference between them, thereby finish remaining in the qualitative work of the liquor smell constituent in the 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; The temperature programme condition: first post, column temperature are initiated with 30 ℃, keep 2min to rise to 80 ℃ with the Cheng Sheng speed of 3 ℃/min, and the speed with 5 ℃/min rises to 255 ℃ again, keeps 32min.Second post, column temperature are initiated with 70 ℃, keep 2.5min to rise to 85 ℃ with the Cheng Sheng speed of 3 ℃/min, and the speed with 5 ℃/min rises to 260 ℃ again, 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 advances automatic processing through the workstation of Pegasus 4D again, and qualitative used spectrogram storehouse is NIST/EPA/NIH Version 2.0.The data obtained draws net result through further processing again.Result such as Fig. 4 and Fig. 5, Fig. 4 are the analysis result figure of liquor 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, does not just add any wine sample in special wineglass.Can clearly contrast from Fig. 4 and Fig. 5, the blank liquid of collecting of liquor gas collection liquor ratio has obviously had more 6 peaks, and what these 6 peaks represented is exactly the constituent that liquor remains in smell in the wineglass.

Claims (6)

1. research remains in the method for the liquor smell in the wineglass, it is characterized in that: may further comprise the steps:
A, in wineglass, add liquor, then leave standstill at least and outwell liquor behind the 3min, then wineglass is left standstill at least 1h at normal temperatures;
B, collection remain in the liquor gas in the wineglass;
C, utilize comprehensive two dimensional gas chromatography-flight mass spectrum that the liquor gaseous matter of collecting is analyzed, and compare with blank sample, thereby determine the constituent that remains in the odoring substance in the wineglass.
2. research as claimed in claim 1 remains in the method for the liquor smell in the wineglass, it is characterized in that: 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, described gas vent is provided with construction of switch on (3), in the A step, described construction of switch is in closed condition; In the B step, the opening switch structure utilizes gas vent (3) to collect the liquor gas that remains in the wineglass.
3. research as claimed in claim 2 remains in the method for the liquor smell in the 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 the B step, utilize push rod (4) pushing piston (5) at the uniform velocity to be pressed into from the opening part of cup (1) so that the liquor gas in the cup (1) from gas vent (3) thus discharge to collect liquor gas.
4. remain in the method for the liquor smell in the wineglass such as claim 1,2 or 3 described researchs, it is characterized in that: in the B step, thereby liquor gas is passed into dissolving collection liquor gas in the ethanol water; In the C step, utilize comprehensive two dimensional gas chromatography-flight mass spectrum respectively the ethanol water and the blank ethanol water that are dissolved with liquor gas to be analyzed contrast, thereby determine the constituent that remains in the odoring substance in the wineglass.
5. research as claimed in claim 4 remains in the method for the liquor smell in the wineglass, it is characterized in that: the ethanol volume ratio of described ethanol water is 55%.
6. remain in the method for the liquor smell in the wineglass such as claim 1,2 or 3 described researchs, it is characterized in that: in the A step, the amount that adds liquor in the wineglass is 10ml, outwells liquor after leaving standstill 10min, dry as far as possible the liquid in the wineglass, then wineglass is left standstill 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 (2)

* 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》 *
赵东等: "气相色谱一质谱法测定酒糟、白酒中的芳香族香味成分", 《酿酒科技》 *

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