CN105300784A - Method for concentrating aromatic components in Wuliangye liquor - Google Patents
Method for concentrating aromatic components in Wuliangye liquor Download PDFInfo
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- CN105300784A CN105300784A CN201510589778.5A CN201510589778A CN105300784A CN 105300784 A CN105300784 A CN 105300784A CN 201510589778 A CN201510589778 A CN 201510589778A CN 105300784 A CN105300784 A CN 105300784A
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Abstract
The invention discloses a method for concentrating aromatic components in Wuliangye liquor. The method comprises the following steps: weighing the Wuliangye liquor, and diluting 100mL of a liquor sample with water till an ethanol content is 10 percent: weighing 4g of sodium chloride, adding the diluted Wuliangye liquor and the sodium chloride into a reaction vessel, adding a mixed solution of methylene dichloride, diethyl ether and pentane, performing continuous extraction, removing water in an organic phase, and filtering with a filter membrane; loading a mixed solution obtained by filtering with the filter membrane in the step (1) into a Vigreux column, putting into a constant-temperature water bath kettle being 45 to 55 DEG C to perform Vigreux fractionation concentration, taking the mixed solution subjected to the Vigreux fractionation concentration out, and concentrating with a pressure blowing concentrator to obtain concentrated aromatic components in the Wuliangye liquor. The method is easy and convenient to operate, time and labor are saved, the cost is low, trace components can be enriched and concentrated, and qualitative and quantitative analysis of extremely trace substances is facilitated. Meanwhile, the losses of volatile components are reduced effectively, and the recovering rates of aromatic substances are increased.
Description
Technical field
The invention belongs to bromatology field, relate to a kind of five-Grain Liquor wine, specifically a kind of method for concentration of five-Grain Liquor wine aroma composition.
Background technology
Fragrance affects one of five-Grain Liquor wine product qualitative factor.By carrying out the analysis of fragrance component to five-Grain Liquor wine, identify the characteristic flavor compounds in wine, the quality improving five-Grain Liquor wine is had great significance.
At present about the fragrance component method for concentration of five-Grain Liquor wine mainly comprises: nitrogen blows method, rotary evaporation, traditional vacuum concentration method and K-D concentration method etc.But these methods cut both ways, owing to employing more organic solvent when white wine extracts, as adopted nitrogen to blow method and rotary evaporation causes the aroma substance of high volatility very easily to escape, micro constitutent is difficult to analyze; Traditional vacuum concentration method and K-D concentration method complex structure, apparatus expensive, complex operation, experiment composition are high.And thorn type fractionating process can make in fragrance concentration process, in rising steam, solvent increases, and the component increase that the condensed fluid mid-boiling point declined is high, if continued repeatedly, just equal to have carried out vapor liquid equilibrium repeatedly, namely achieve and repeatedly distill, finally at still top, solvent is discharged, effectively can improve the concentrated effect of fragrance.
Summary of the invention
For the problems referred to above of the prior art, the invention provides a kind of method for concentration of five-Grain Liquor wine aroma composition, the method for concentration of described this five-Grain Liquor wine aroma composition solves that aroma substance in the method for concentrated five-Grain Liquor wine aroma composition of the prior art easily loses, micro constitutent is difficult to analysis operation loaded down with trivial details experiment composition high-technology problem.
The invention provides a kind of method for concentration of five-Grain Liquor wine aroma composition, comprise the steps:
1) one adopts the step of complex solvent extraction, first measure five-Grain Liquor wine, being diluted with water to ethanol content is 10%, wine sample is diluted: the ratio of 4g sodium chloride takes sodium chloride according to 100mL, the five-Grain Liquor wine of dilution, sodium chloride are joined in a reaction vessel, add methylene chloride, ether and pentane mixed liquor again, continuous extraction 3-5 time, by organic phase centrifugal 10-20 minute under 3000-4000r/min condition, get upper organic phase, by the moisture removing in organic phase, then adopt membrane filtration;
2) step adopting thorn type fractionation plant concentrated, the mixed solution obtained after step (1) membrane filtration is loaded thorn type fractionation plant, be positioned in the thermostat water bath of 45-55 DEG C and carry out thorn type fractional condensation, the mixed liquor Nitrogen evaporator taken out after thorn type fractional condensation concentrates, and obtains the five-Grain Liquor wine aroma composition after concentrating.
Further, in described methylene chloride, ether and pentane mixed liquor, the volume ratio of methylene chloride, ether and pentane is 7:2:1.
Further, the aperture of described filter membrane is 0.22 μm.
Further, in organic phase, add anhydrous sodium sulfate removing moisture.
Present invention employs a kind of method for concentration of fragrance component, effect that is concentrated, enrichment can be played to the microcomponent in five-Grain Liquor wine.Thorn type still just has one group of downward-sloping thorn every a segment distance, and the fractionating column arranged in the shape of a spiral between each group thorn.In still, when the condensed fluid of steam and the decline of rising coagulate mutually contact time, the condensed fluid partial gasification that heat makes decline is released in the vapor portion condensation of rising, and there occurs exchange heat between the two, and solvent in rising steam is increased, and the component increase that the condensed fluid mid-boiling point declined is high, if continued repeatedly, just equal to have carried out vapor liquid equilibrium repeatedly, namely achieve and repeatedly distill, finally at still top, solvent is discharged, reach the effect of concentrating sample.This process decreases the component damages in mixed liquor, thus reflects the contamination of the volatile matter in sample more really.
The present invention compares with prior art, and its technical progress is significant.The invention provides a kind of method for concentration of five-Grain Liquor wine aroma composition, by selecting suitable solvent and method for concentration volatile ingredient extracted and concentrate, obtaining more fully volatile ingredient and more real content of material.The present invention is simple, convenient, time saving and energy saving, low cost, enrichment, concentrated effect can be played to microcomponent, the qualitative analysis that accessory substance is few, be conducive to denier material, effectively reduces the loss of volatile ingredient simultaneously, improves the recovery of aroma substance.
Accompanying drawing explanation
Fig. 1 shows commercially available five-Grain Liquor wine aroma composition chromatogram.
Embodiment
Embodiment 1
1) complex solvent extraction: get a kind of commercially available five-Grain Liquor wine (50% alcoholic strength) 25mL, add the dilution of 100mL water, add 5g sodium chloride again, add methylene chloride, ether and pentane mixed liquor (volume ratio 7:2:1) successively, respectively methylene chloride, ether and pentane mixed liquor 20mL, 20mL, 20mL continuous extraction three times, by organic phase under 3000r/min condition centrifugal 20 minutes, get upper organic phase, anhydrous sodium sulfate removing moisture is added again, the dewatered organic phase membrane filtration of 0.22 μm in organic phase;
2) thorn type fractional condensation: the step of a thorn type fractional condensation, in the step of described thorn type fractional condensation, the mixed solution obtained after step (1) membrane filtration is loaded cucurbit, be positioned in the thermostat water bath of 45 DEG C and carry out thorn type fractional condensation, solvent and a small amount of effumability composition enter into thorn type fractionating column, when in bottle to be distilled, solution has steamed substantially, remove water-bath, volatile components cools in thorn type fractionating column to be got back in cucurbit, drop is no longer included when dripping in type fractionating column cocked, after taking-up mixed liquor Nitrogen evaporator is concentrated into 1mL, the octyl propionate solution adding 800 μ L1g/L is internal standard compound, mixing treats that GC-MS analyzes.
3) the concentrate direct injected of getting 1 this embodiment 1 of μ L carries out GC-MS analysis.Select 7890-5975 gas chromatograph-mass spectrometer, GC condition is: capillary chromatographic column is AgilentHP-INNOWAX (60m × 0.25mm × 0.25 μm) injector temperature 230 DEG C, temperature programme: initial temperature 40 DEG C, retain 6min, 100 DEG C are risen to the speed of 3 DEG C/min, rise to 230 DEG C with the speed of 5 DEG C/min again, keep 20min; Detector temperature 230 DEG C; Carrier gas He, flow velocity is 1mL/min; Split ratio 10:1 sample introduction; MS condition: quadrupole rod temperature 150 DEG C, ion source temperature 230 DEG C, interface temperature 280 DEG C, EI ionization source, electron energy 70ev, sweep limit, 30 ~ 400amu.
4) qualitative and quantitative analysis of volatile ingredient: the mass spectrum of unknown compound is by comparing with wiley7nDatabase, NIST05 (AgilentTechnologiesInc.); And it is qualitative further by calculating retention index; Internal standard method is adopted to carry out quantitatively, computing formula:
in formula, fi correction factor is 1, Ai component peaks area to be measured, the peak area of As internal standard compound, the quality of Ws internal standard compound, Ni test substance quality.
By fragrance method for concentration of the present invention, identify 86 kinds of fragrance components altogether, fragrance component total content is 1611.889mg/L; And only blow method for concentration by nitrogen, identify 76 kinds of fragrance components altogether, fragrance component total content is 1510.039mg/L.
As can be seen here, the aroma substance kind that fragrance method for concentration of the present invention identifies and total content blow higher than nitrogen the kind and content that method for concentration identifies, this invention can reflect aroma substance composition and content in five-Grain Liquor wine more accurately.The testing result of table 1 for adopting method of the present invention and traditional nitrogen to blow the five-Grain Liquor wine aroma composition that method obtains.
The testing result (example 1) of table 1 five-Grain Liquor wine aroma composition
Embodiment 2
1) complex solvent extraction: get a kind of commercially available five-Grain Liquor wine (50% alcoholic strength) 25mL, add the dilution of 100mL water, add 5g sodium chloride again, add methylene chloride, ether and pentane mixed liquor (volume ratio 7:2:1) successively, respectively methylene chloride, ether and pentane mixed liquor 20mL, 20mL, 20mL, 20mL, 20mL continuous extraction five times, by organic phase under 3500r/min condition centrifugal 10 minutes, get upper organic phase, anhydrous sodium sulfate removing moisture is added again, the dewatered organic phase membrane filtration of 0.22 μm in organic phase;
2) thorn type fractional condensation: the step of a thorn type fractional condensation, in the step of described thorn type fractional condensation, the mixed solution obtained after step (1) membrane filtration is loaded cucurbit, be positioned in the thermostat water bath of 50 DEG C and carry out thorn type fractional condensation, solvent and a small amount of effumability composition enter into thorn type fractionating column, when in bottle to be distilled, solution has steamed substantially, remove water-bath, volatile components cools in thorn type fractionating column to be got back in cucurbit, drop is no longer included when dripping in type fractionating column cocked, after taking-up mixed liquor Nitrogen evaporator is concentrated into 1mL, the octyl propionate solution adding 800 μ L1g/L is internal standard compound, mixing treats that GC-MS analyzes.
3) the concentrate direct injected of getting 1 this embodiment 1 of μ L carries out GC-MS analysis.Select 7890-5975 gas chromatograph-mass spectrometer, GC condition is: capillary chromatographic column is AgilentHP-INNOWAX (60m × 0.25mm × 0.25 μm) injector temperature 230 DEG C, temperature programme: initial temperature 40 DEG C, retain 6min, 100 DEG C are risen to the speed of 3 DEG C/min, rise to 230 DEG C with the speed of 5 DEG C/min again, keep 20min; Detector temperature 230 DEG C; Carrier gas He, flow velocity is 1mL/min; Split ratio 10:1 sample introduction; MS condition: quadrupole rod temperature 150 DEG C, ion source temperature 230 DEG C, interface temperature 280 DEG C, EI ionization source, electron energy 70ev, sweep limit, 30 ~ 400amu.
4) qualitative and quantitative analysis of volatile ingredient: the mass spectrum of unknown compound is by comparing with wiley7nDatabase, NIST05 (AgilentTechnologiesInc.); And it is qualitative further by calculating retention index; Internal standard method is adopted to carry out quantitatively, computing formula:
in formula, fi correction factor is 1, Ai component peaks area to be measured, the peak area of As internal standard compound, the quality of Ws internal standard compound, Ni test substance quality.
By fragrance method for concentration of the present invention, identify 72 kinds of fragrance components altogether, fragrance component total content is 2017.850mg/L; And only blow method for concentration by nitrogen, identify 63 kinds of fragrance components altogether, fragrance component total content is 1911.983mg/L.
As can be seen here, the aroma substance kind that fragrance method for concentration of the present invention identifies and total content blow higher than nitrogen the kind and content that method for concentration identifies, this invention can reflect aroma substance composition and content in five-Grain Liquor wine more accurately.The testing result of table 2 for adopting method of the present invention and traditional nitrogen to blow the five-Grain Liquor wine aroma composition that method obtains.
The testing result (example 2) of table 2 five-Grain Liquor wine aroma composition
Embodiment 3
1) complex solvent extraction: get a kind of commercially available five-Grain Liquor wine (50% alcoholic strength) 25mL, add the dilution of 100mL water, add 5g sodium chloride again, add methylene chloride, ether and pentane mixed liquor (volume ratio 7:2:1) successively, respectively methylene chloride, ether and pentane mixed liquor 20mL, 20mL, 20mL, 20mL continuous extraction four times, by organic phase under 4000r/min condition centrifugal 15 minutes, get upper organic phase, anhydrous sodium sulfate removing moisture is added again, the dewatered organic phase membrane filtration of 0.22 μm in organic phase;
2) thorn type fractional condensation: the step of a thorn type fractional condensation, in the step of described thorn type fractional condensation, the mixed solution obtained after step (1) membrane filtration is loaded cucurbit, be positioned in the thermostat water bath of 55 DEG C and carry out thorn type fractional condensation, solvent and a small amount of effumability composition enter into thorn type fractionating column, when in bottle to be distilled, solution has steamed substantially, remove water-bath, volatile components cools in thorn type fractionating column to be got back in cucurbit, drop is no longer included when dripping in type fractionating column cocked, after taking-up mixed liquor Nitrogen evaporator is concentrated into 1mL, the octyl propionate solution adding 800 μ L1g/L is internal standard compound, mixing treats that GC-MS analyzes.
3) the concentrate direct injected of getting 1 this embodiment 1 of μ L carries out GC-MS analysis.Select 7890-5975 gas chromatograph-mass spectrometer, GC condition is: capillary chromatographic column is AgilentHP-INNOWAX (60m × 0.25mm × 0.25 μm) injector temperature 230 DEG C, temperature programme: initial temperature 40 DEG C, retain 6min, 100 DEG C are risen to the speed of 3 DEG C/min, rise to 230 DEG C with the speed of 5 DEG C/min again, keep 20min; Detector temperature 230 DEG C; Carrier gas He, flow velocity is 1mL/min; Split ratio 10:1 sample introduction; MS condition: quadrupole rod temperature 150 DEG C, ion source temperature 230 DEG C, interface temperature 280 DEG C, EI ionization source, electron energy 70ev, sweep limit, 30 ~ 400amu.
4) qualitative and quantitative analysis of volatile ingredient: the mass spectrum of unknown compound is by comparing with wiley7nDatabase, NIST05 (AgilentTechnologiesInc.); And it is qualitative further by calculating retention index; Internal standard method is adopted to carry out quantitatively, computing formula:
in formula, fi correction factor is 1, Ai component peaks area to be measured, the peak area of As internal standard compound, the quality of Ws internal standard compound, Ni test substance quality.
By fragrance method for concentration of the present invention, identify 82 kinds of fragrance components altogether, fragrance component total content is 1627.963mg/L; And only blow method for concentration by nitrogen, identify 71 kinds of fragrance components altogether, fragrance component total content is 1419.022mg/L.
As can be seen here, the aroma substance kind that fragrance method for concentration of the present invention identifies and total content blow higher than nitrogen the kind and content that method for concentration identifies, this invention can reflect aroma substance composition and content in five-Grain Liquor wine more accurately.The testing result of table 3 for adopting method of the present invention and traditional nitrogen to blow the five-Grain Liquor wine aroma composition that method obtains.
The testing result (example 3) of table 3 five-Grain Liquor wine aroma composition
Claims (4)
1. a method for concentration for five-Grain Liquor wine aroma composition, is characterized in that comprising the steps:
1) one adopts the step of complex solvent extraction, first measure five-Grain Liquor wine, being diluted with water to ethanol content is 10%, wine sample is diluted: the ratio of 4g sodium chloride takes sodium chloride according to 100mL, the five-Grain Liquor wine of dilution, sodium chloride are joined in a reaction vessel, add methylene chloride, ether and pentane mixed liquor again, continuous extraction 3-5 time, by organic phase centrifugal 10-20 minute under 3000-4000r/min condition, get upper organic phase, by the moisture removing in organic phase, then adopt membrane filtration;
2) step adopting thorn type fractionation plant concentrated, the mixed solution obtained after step (1) membrane filtration is loaded thorn type fractionation plant, be positioned in the thermostat water bath of 45-55 DEG C and carry out thorn type fractional condensation, the mixed liquor Nitrogen evaporator taken out after thorn type fractional condensation concentrates, and obtains the five-Grain Liquor wine aroma composition after concentrating.
2. the method for concentration of a kind of five-Grain Liquor wine aroma composition according to claim 1, is characterized in that: in described methylene chloride, ether and pentane mixed liquor, and the volume ratio of methylene chloride, ether and pentane is 7:2:1.
3. the method for concentration of a kind of five-Grain Liquor wine aroma composition according to claim 1, is characterized in that: the aperture of described filter membrane is 0.22 μm.
4. the method for concentration of a kind of five-Grain Liquor wine aroma composition according to claim 1, is characterized in that: in organic phase, add anhydrous sodium sulfate removing moisture.
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| CN109374759A (en) * | 2018-09-12 | 2019-02-22 | 北京工商大学 | A kind of method for concentration based on white wine liquid-liquid extraction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675159A (en) * | 2013-11-26 | 2014-03-26 | 浙江大学 | Simultaneous distillation-extraction detection method of volatile flavor substances in sour-dough steamed bun |
| CN104596833A (en) * | 2015-01-19 | 2015-05-06 | 上海应用技术学院 | Method for concentrating volatile components in kirschwasser |
-
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675159A (en) * | 2013-11-26 | 2014-03-26 | 浙江大学 | Simultaneous distillation-extraction detection method of volatile flavor substances in sour-dough steamed bun |
| CN104596833A (en) * | 2015-01-19 | 2015-05-06 | 上海应用技术学院 | Method for concentrating volatile components in kirschwasser |
Non-Patent Citations (1)
| Title |
|---|
| 刘淑琴 等: "酒类香气物质研究进展", 《食品工业科技》 * |
Cited By (1)
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|---|---|---|---|---|
| CN109374759A (en) * | 2018-09-12 | 2019-02-22 | 北京工商大学 | A kind of method for concentration based on white wine liquid-liquid extraction |
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