CN105241738A - Concentration method for apple-flavor cocktail fragrance ingredient - Google Patents
Concentration method for apple-flavor cocktail fragrance ingredient Download PDFInfo
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- CN105241738A CN105241738A CN201510589000.4A CN201510589000A CN105241738A CN 105241738 A CN105241738 A CN 105241738A CN 201510589000 A CN201510589000 A CN 201510589000A CN 105241738 A CN105241738 A CN 105241738A
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Abstract
A concentration method for an apple-flavor cocktail fragrance ingredient comprises weighing apple-flavor cocktail and putting in a container, adding sodium chloride to enable the solution to be at a saturated salt solution state, so as to obtain a to-be extracted solution; adding a mixed solution of dichloromethane, ether and pentane into the prepared to-be extracted solution, performing continuous extraction, getting the upper layer organic phase, removing water in the organic phase, and then filtering by a filter membrane; adding a mixed solution, which is obtained after filter-film filtering is performed, into a vigreux fractionation apparatus, putting into a 40-50 DEG C constant-temperature water bath pot for vigreus fractionation concentration, getting a mixed solution subjected to vigreus fractionation concentration, and then concentrating by using a nitrogen blowing instrument, so as to obtain the concentrated apple-flavor cocktail fragrance ingredient. The method is simple and convenient in operation, time-saving, labor-saving and low in cost, gives play to enriching and concentrating effects on trace compositions, is beneficial for qualitative quantitative analysis on infinitesimal substances, and also helps to effectively reduce loss of volatile compositions and improve recovery rate of the fragrance substance.
Description
Technical field
The invention belongs to bromatology field, especially a kind of apple aroma cocktail is fragrant, a kind of method for concentration of apple aroma cocktail fragrance component specifically.
Background technology
Fragrance affects one of cocktail product qualitative factor.By carrying out the analysis of fragrance component to apple aroma cocktail, identify characteristic flavor compounds, the cocktail quality of raising is had great significance.
At present about cocktail fragrance component method for concentration 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 tealeaves 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 apple aroma cocktail fragrance component, the method for concentration of described this apple aroma cocktail fragrance component solve concentrated cocktail fragrance component of the prior art method aroma substance easily loses, micro constitutent is difficult to analysis, complex operation, experiment composition high-technology problem.
The invention provides a kind of method for concentration of apple aroma cocktail fragrance component, comprise the steps:
1) one adopts the step of complex solvent extraction, measure apple aroma cocktail in a container, adding sodium chloride to it is saturated salt solution state, obtain liquid to be extracted, add methylene chloride, ether and pentane mixed liquor by ready liquid to be extracted, continuous extraction 2-4 time, by organic phase centrifugal 10-20 minute under 3000-4000r/min condition, get upper organic phase, in organic phase, remove moisture, then membrane filtration;
2) step adopting thorn type fractionation plant concentrated, the mixed solution obtained after step (1) membrane filtration is added in thorn type fractionation plant, be positioned in the thermostat water bath of 40-50 DEG C and carry out thorn type fractional condensation, take out the mixed liquor after thorn type fractional condensation, then concentrate with Nitrogen evaporator, obtain after concentrating
Apple aroma cocktail fragrance component.
Further, in described methylene chloride, ether and pentane mixed liquor, the volume ratio of methylene chloride, ether and pentane is 1:1:1.
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 apple aroma cocktail.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 cocktail fragrance component, 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 apple aroma cocktail fragrance component chromatogram.
Embodiment
Embodiment 1
1) complex solvent extraction: get commercially available apple aroma cocktail 100mL in sample bottle, adding analysis pure sodium chloride is saturated salt solution state to it, obtains liquid to be extracted.Methylene chloride, ether and pentane mixed liquor is added by ready liquid to be extracted, continuous extraction 3 times, by organic phase under 3500r/min condition centrifugal 15 minutes, gets upper organic phase, anhydrous sodium sulfate removing moisture is added again, dewatered organic phase membrane filtration 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 (2) membrane filtration is loaded cucurbit, be positioned in the thermostat water bath of 40 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 is concentrated with Nitrogen evaporator, the sec-n-octyl alcohol solution (diluting with ethanol) adding 160 μ L400mg/L is internal standard compound, and 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 10min; Detector temperature 230 DEG C; Carrier gas He, flow velocity is 1.2mL/min; Splitless injecting samples; 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 66 kinds of fragrance components altogether, fragrance component total content is 70.779mg/L; ; And only blow method for concentration by nitrogen, identify 46 kinds of fragrance components altogether, fragrance component total content is 63.770mg/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 apple aroma cocktail more accurately.The testing result of table 1 for adopting method of the present invention and traditional nitrogen to blow the cocktail fragrance component that method obtains.
The testing result (example 1) of table 1 apple aroma cocktail fragrance component
ND: do not detect
Embodiment 2
1) complex solvent extraction: get commercially available apple aroma cocktail 100mL in sample bottle, adding analysis pure sodium chloride is saturated salt solution state to it, obtains liquid to be extracted.Methylene chloride, ether and pentane mixed liquor is added by ready liquid to be extracted, continuous extraction 2 times, by organic phase under 3000r/min condition centrifugal 10 minutes, gets upper organic phase, anhydrous sodium sulfate removing moisture is added again, dewatered organic phase membrane filtration 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 is concentrated with Nitrogen evaporator, the sec-n-octyl alcohol solution (diluting with ethanol) adding 160 μ L400mg/L is internal standard compound, and mixing treats that GC-MS analyzes.
All the other analysis conditions are with reference to example 1.
By the fragrance method for concentration of this example, identify 64 kinds of fragrance components altogether, fragrance component total content is 64.986mg/L; And only blow method for concentration by nitrogen, identify 49 kinds of fragrance components altogether, fragrance component total content is 60.231mg/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 apple aroma cocktail more accurately.The testing result of table 2 for adopting method of the present invention and traditional nitrogen to blow the cocktail fragrance component that method obtains.
The testing result (example 2) of table 2 apple aroma cocktail fragrance component
ND: do not detect
Embodiment 3
1) complex solvent extraction: get commercially available apple aroma cocktail 100mL in sample bottle, adding analysis pure sodium chloride is saturated salt solution state to it, obtains liquid to be extracted.Methylene chloride, ether and pentane mixed liquor is added by ready liquid to be extracted, continuous extraction 4 times, by organic phase under 4000r/min condition centrifugal 20 minutes, gets upper organic phase, anhydrous sodium sulfate removing moisture is added again, dewatered organic phase membrane filtration 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 is concentrated with Nitrogen evaporator, the sec-n-octyl alcohol solution (diluting with ethanol) adding 160 μ L400mg/L is internal standard compound, and mixing treats that GC-MS analyzes.
All the other analysis conditions are with reference to example 1.
By the fragrance method for concentration of this example, identify 64 kinds of fragrance components altogether, fragrance component total content is 64.490mg/L; And only blow method for concentration by nitrogen, identify 52 kinds of fragrance components altogether, fragrance component total content is 62.012mg/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 apple aroma cocktail more accurately.The testing result of table 3 for adopting method of the present invention and traditional nitrogen to blow the cocktail fragrance component that method obtains.
The testing result (example 3) of table 3 apple aroma cocktail fragrance component
ND: do not detect.
Claims (4)
1. a method for concentration for apple aroma cocktail fragrance component, is characterized in that comprising the steps:
1) one adopts the step of complex solvent extraction, measure apple aroma cocktail in a container, adding sodium chloride to it is saturated salt solution state, obtain liquid to be extracted, add methylene chloride, ether and pentane mixed liquor by ready liquid to be extracted, continuous extraction 2-4 time, by organic phase centrifugal 10-20 minute under 3000-4000r/min condition, get upper organic phase, in organic phase, remove moisture, then membrane filtration;
2) step adopting thorn type fractionation plant concentrated, the mixed solution obtained after step (1) membrane filtration is added in thorn type fractionation plant, be positioned in the thermostat water bath of 40-50 DEG C and carry out thorn type fractional condensation, take out the mixed liquor after thorn type fractional condensation, then concentrate with Nitrogen evaporator, obtain the apple aroma cocktail fragrance component after concentrating.
2. the method for concentration of a kind of apple aroma cocktail fragrance component 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 1:1:1.
3. the method for concentration of a kind of apple aroma cocktail fragrance component 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 apple aroma cocktail fragrance component according to claim 1, is characterized in that: in organic phase, add anhydrous sodium sulfate removing moisture.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784875A (en) * | 2016-05-11 | 2016-07-20 | 北京工商大学 | Pretreatment method and detection method for analysis on ingredients in liquor |
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| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| 刘淑琴 等: "酒类香气物质研究进展", 《食品工业科技》 * |
| 梁忠英: "《化工原理》", 31 August 2002, 中国医药科技出版社，第1版 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784875A (en) * | 2016-05-11 | 2016-07-20 | 北京工商大学 | Pretreatment method and detection method for analysis on ingredients in liquor |
| CN105784875B (en) * | 2016-05-11 | 2018-07-24 | 北京工商大学 | A kind of pre-treating method and detection method for constituent analysis in white wine |
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Application publication date: 20160113 |