CN103146517B - Method for extracting high-ester seasoning liquid from after-run - Google Patents
Method for extracting high-ester seasoning liquid from after-run Download PDFInfo
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- CN103146517B CN103146517B CN201210189220.4A CN201210189220A CN103146517B CN 103146517 B CN103146517 B CN 103146517B CN 201210189220 A CN201210189220 A CN 201210189220A CN 103146517 B CN103146517 B CN 103146517B
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- 239000007788 liquid Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 22
- 235000011194 food seasoning agent Nutrition 0.000 title abstract 7
- 238000000855 fermentation Methods 0.000 claims abstract description 17
- 230000004151 fermentation Effects 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 12
- 235000014101 wine Nutrition 0.000 claims description 78
- 238000000605 extraction Methods 0.000 claims description 35
- 150000002148 esters Chemical class 0.000 claims description 22
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 16
- 235000015096 spirit Nutrition 0.000 claims description 12
- 229940074391 gallic acid Drugs 0.000 claims description 8
- 235000004515 gallic acid Nutrition 0.000 claims description 8
- 235000007164 Oryza sativa Nutrition 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 235000009566 rice Nutrition 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 3
- 230000001351 cycling effect Effects 0.000 claims description 3
- 238000007667 floating Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- 238000013517 stratification Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 abstract description 32
- 235000014113 dietary fatty acids Nutrition 0.000 abstract description 8
- 229930195729 fatty acid Natural products 0.000 abstract description 8
- 239000000194 fatty acid Substances 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000000796 flavoring agent Substances 0.000 abstract description 4
- 235000019634 flavors Nutrition 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 3
- 239000003205 fragrance Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000000194 supercritical-fluid extraction Methods 0.000 description 8
- 239000000284 extract Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000000470 constituent Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 241000209094 Oryza Species 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 235000011089 carbon dioxide Nutrition 0.000 description 4
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- XIRNKXNNONJFQO-UHFFFAOYSA-N ethyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCC XIRNKXNNONJFQO-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 235000020097 white wine Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 229940116333 ethyl lactate Drugs 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012470 diluted sample Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 229940067592 ethyl palmitate Drugs 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000010563 solid-state fermentation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for extracting a high-ester seasoning liquid from after-run and belongs to the field of recovering a white spirit fermentation by-product. The method comprises the following steps of selecting after-run raw materials, pretreating the after-run raw materials and extracting and separating the high-ester seasoning liquid. The high-ester seasoning liquid is complex liquid comprising a plurality of flavor components such as ethyl caproate as a main flavor component, has the advantages of high ethyl caproate content above 250g/L, low long-chain higher fatty acid ethyl ester content, no color, transparent character, and thick, pure and appropriate fragrance, and can be used for white spirit blending thereby obviously improving white spirit quality. The high-ester seasoning liquid is extracted from after-run obtained by special material selection of a white spirit fermentation by-product. In the whole method, the high-ester seasoning liquid does not contact with any chemical reagents and is a natural seasoning liquid.
Description
Technical field
The present invention relates to the separating and extracting method of a kind of wine high-ester flavouring liquid, belong to the recovery field of liquor fermentation by product.
Background technology
Wine tail is that conventional solid-state white liquor distilling process is interrupted the low alcohol that Hua Housuo plucks, and alcoholic strength generally, between 14～20 °, contains a large amount of esters of gallic acid compositions in wine tail.Most brewery still adopts returns wine tail to the mode that end pot string steams, and extracts remaining part alcohol and part esters of gallic acid material in wine tail.This traditional way exist damage wine, only can Extraction parts the also drawback such as volatile acid Ester, a large amount of beneficiating ingredients in wine tail still can not effectively be extracted.Indivedual producers have adopted supercritical extraction mode to extract the effective constituent in wine tail.As wine tail is first carried out rectifying by patent CN100415866C, obtain the rectifying still liquid that ethanol content is extremely low, and then adopt supercritical extraction mode to extract beneficiating ingredient wherein this mixed solution, but its shortcoming is extracted component is high boiling point organic compound mostly, the not skeletal substance such as the acid esters in white wine, and component concentration is lower.
In traditional aroma daqu liquor is produced, vinosity improves by the mode that extends fermentation period in most families that produce, extend fermentation period and can improve product ester ability in cellar for storing things, especially very high near the content of Ester in the wine unstrained spirits of a rice steamer at the bottom of pond, and then the content that distills the Ester in former wine is raise, fermentation time is longer, and the Ester in the former wine especially content of ethyl hexanoate is just higher.But by distillation, only can extract the ester class of a small part, most Ester is dissolved in wine tail or remains in poor unstrained spirits.Find through observing, fermentation period was at the Jiao Chi of 4～6 months, wine tail warp near the rice steamer wine unstrained spirits at the bottom of pond leaves standstill a night, and wine tail surface can produce a large amount of oily matter, and this oily matter contains the materials such as a large amount of ethyl hexanoates, caproic acid and ethyl palmitate after testing.If but with this oily matter wine blending, owing to there being the existence of higher fatty acid ethyl esters, be easy to make wine body muddiness.
That supercritical carbon dioxide extraction method has is pure, safety, no solvent residue, extraction yield is high, flow process is simple, solvent carbonic acid gas relative low price and the plurality of advantages such as can be recycled, and is widely used in food medicine and other fields.The stagnation point of carbonic acid gas is 31.06 DEG C, 7.39Mp, and its critical temperature and pressure are all lower, be easy to industrialization, and the advantage such as that carbonic acid gas has is non-combustible, nontoxic, chemical stability is good, easily separated, cheap and easy to get, is therefore widely used in supercritical extraction process.The density of supercritical carbon dioxide fluid can regulate by changing pressure, the change of density directly affects its dissolving power, therefore supercritical extraction can be with the dissolving power of pressure control supercutical fluid, i.e. extracting effective components or remove objectionable constituent selectively.Carbonic acid gas is a kind of non-polar solvent, for nonpolar small-molecule substance, as the volatile small molecule materials such as the lower aliphatic acetoacetic esters such as ethyl hexanoate, ethyl lactate, ethyl acetate and alcohol, caproic acid, butyric acid have higher extraction yield, for the larger acidic substance of polarity or macromolecular substance, as higher fatty acid ethyl esters etc., extraction yield is very low.Therefore can selectively extract needed effective constituent by the control of supercritical process parameter.
Summary of the invention
The object of this invention is to provide a kind of method of extracting high-ester flavouring liquid from wine tail, utilize the method from this special wine tail, to extract the high Wine blending liquid of ethyl hexanoate content, this Wine blending liquid ethyl hexanoate content is high, reaches 250g/L; Higher fatty acid ethyl esters content is few, is applicable to hook adjust low and middle-grade white wine, not only can not produce muddiness, and cellar for storing things is fragrant pure, has the typical style of aromatic Chinese spirit.
The present invention extracts the method for wine high-ester flavouring liquid from wine tail, comprises the steps:
(1) selection of wine tail: selecting wine unstrained spirits fermentation period is the aromatic Chinese spirit fermentation pit of 4 to 6 months, and select the wine unstrained spirits dividing near bottom, Jiao Chi pond, wine unstrained spirits obtains the lower concentration wine tail of alcoholic strength in 15%～20% scope through the distillation of rice steamer bucket.
(2) pre-treatment step of wine tail: by above-mentioned selected low boilers for low-proof wine stratification, collect the floating oily matter in wine tail upper strata, obtain wine tail oily matter;
(3) extraction step: the wine tail oily matter of step 2 is placed in to supercritical CO
2extraction kettle in, regulating extraction kettle pressure is 7.5～8Mp, extraction kettle temperature is 35～45 DEG C; Extraction time is 1h～2h; Make esters of gallic acid material in wine tail be dissolved in supercritical CO
2in fluid;
(4) separating step: will carry the CO of esters of gallic acid material in step (3)
2fluid successively enters separating still I and separating still II; Described separating still I pressure is 6.5～7Mp, and separating still I temperature is 35～40 DEG C; Separating still II pressure is 4.5～5Mp, and separating still II temperature is 25～35 DEG C, by reducing CO in separating still
2pressure, esters of gallic acid material is resolved in separating still; The parsing thing of collecting separating still II, this parsing thing is colourless transparent liquid, is high-ester flavouring liquid.
The parsing thing obtaining in separating still I in described step (4) is forwarded to and in extraction kettle, carries out cycling extraction separation; To reach the high efficiente callback of active principle.
Foundation of the present invention and principle: the selected wine tail of the present invention be fermentation period the wine tail in the Chang Jiao pond of 4～6 months and only at the bottom of scavenger wine unstrained spirits be object through the low boilers for low-proof wine of rice steamer bucket distillation.Thereby can improve and in cellar for storing things, produce ester ability and improve vinosity owing to extending fermentation period, and the closer at the bottom of pond, in wine unstrained spirits, the content of ester is just higher, especially the content of ethyl hexanoate is just higher.But by distillation, only have part Ester to steam in former wine, most of flavour ingredient steams with wine tail.
The alcohol number of degrees in general wine tail are 20 ° of left and right, and the component that in wine tail, content is maximum is ethyl lactate, and content can reach 10g/L left and right; The less ethyl hexanoate of content is because solubleness in the alcohol of 20 ° of left and right is extremely low, thereby with other hydrophobic components together slowly polymerization, separates out gradually, and floats on the water surface.This part material is wine tail oily matter.This oily matter is taking ethyl hexanoate, caproic acid as main component, but still contain the long-chain component such as a large amount of ethyl palmitates, be directly used in to hook and adjust low and middle-grade wine, because the impact of long-chain fat acetoacetic ester causes wine body muddiness, and assorted taste is outstanding, and this precious resources cannot be applied.For addressing this problem, the present invention utilizes supercritical extraction process to remove higher fatty acid ethyl esters.Ethyl hexanoate and higher fatty acid ethyl esters molecular weight differ larger in theory, thereby this two classes material is at supercritical CO
2in solubleness also there is difference, according to this characteristic, by supercritical extraction method, ethyl hexanoate is separated with higher fatty acid ethyl esters; Thereby obtain the ethyl hexanoate Wine blending liquid of high density.
Therefore, the present invention chooses the Jiao Chi that the solid state fermentation cycle grows, and it is high that such Jiao Chi produces ester content, and wine tail oily matter is more; Adopt supercritical CO
2extraction process is removed objectionable constituent in wine tail oily matter, retains beneficiating ingredient, makes in extraction liquid more than ethyl hexanoate content reaches 250g/L, and extraction liquid water white transparency, vinosity is strong, and the pure coordination of fragrance can significantly promote the quality of white wine for wine blending.This high-ester flavouring liquid extracts and obtains from wine tail, is natural microbial fermentation product, adopts again supercritical extraction process, has advantages of pure, safety, no solvent residue, meets the needs of food safety.
Brief description of the drawings
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is supercritical extraction process schema.
Fig. 3 A-C is the gas chromatographic analysis figure of high-ester flavouring liquid after diluting 100 times.
Embodiment
Below in conjunction with accompanying drawing and example, the present invention is described in further detail:
Embodiment: extract the method for high-ester flavouring liquid the wine tail of producing compared with Chang Jiao pond from fermentation period, carry out as follows:
(1) selection of wine tail: select fermentation period grow the Jiao Chi of (being generally 4 months to 6 months), and to select at the bottom of close pond wine unstrained spirits to distill through rice steamer bucket the low boilers for low-proof wine of plucking be object; Alcoholic strength is generally 15%～20%.
(2) pre-treatment step of wine tail: plucked special wine tail is placed in to storage tank and leaves standstill a night, the floating oily matter in wine tail upper strata in storage tank is collected, obtain wine tail oily matter.
(3) extracting and separating step: adopt supercritical CO
2(this device comprises CO to extraction plant
2, the part composition such as ice chest storage tank, high-pressure pump) heavy constituent (higher fatty acid ethyl esters) to wine tail oily matter separates with light constituent (own ester, caproic acid etc.); As shown in Figure 2, the wine tail oily matter of step 2 is placed in to supercritical CO
2extraction kettle in, regulating extraction kettle pressure is 7.5～8Mp, extraction kettle temperature is 35～45 DEG C; Separating still I pressure is 6.5～7Mp, and separating still I temperature is 35～40 DEG C; Separating still II pressure is 4.5～5Mp, and separating still II temperature is 25～35 DEG C.Extraction time is 1h～2h.
(4) high-ester flavouring liquid (4) high-ester flavouring liquid is collected step: after extraction finishes, open the valve of separating still II, collect the parsing thing of separating still II, this parsing thing is colourless transparent liquid, is the high-ester flavouring liquid taking ethyl hexanoate as main ingredient.This high-ester flavouring liquid water white transparency, extraction yield is more than 10%, and each component concentration is as shown in table 1.This extracting solution adopts gas-chromatography detection method, the CP-WAX57CB capillary column 50m × 0.25mm × 0.20 μ m that Varian Chrompack company of its chromatographic column adopting U.S. produces.Column temperature: second order temperature programming, 35 DEG C of initial temperatures, keep 2 min, be raised to 100 DEG C, then be raised to 210 DEG C with 10 DEG C/min with 4 DEG C/min, keep 15 min; 230 DEG C of injector temperatures; 240 DEG C of detector temperatures; Carrier gas: High Purity Nitrogen; Column cap is pressed: 120 kPa; Post flow: 1.0 mL/min; Sample size: 1 μ L, Fig. 3 A-C is the gas chromatographic analysis figure of high-ester flavouring liquid after diluting 100 times, in figure, from the left side, first large peak value is the etoh solvent peak that diluted sample is used, and the 2nd large peak value is ethyl hexanoate peak, and the 3rd large peak value is caproic acid peak.
(5) extract remainder is collected step: after extraction finishes, open the valve of extraction kettle, collect the raffinate of extraction kettle, this extraction liquid color is scarlet, makes liquid waste disposal, enters anaerobic methane fermentation vat.
(6) recycling step of the parsing thing of separating still I: after extraction time arrives, open the valve of separating still I, collect the parsing thing of separating still I, in this parsing thing, still contain the flavour ingredients such as a large amount of ethyl hexanoates, this is resolved to thing squeezes into extraction kettle again from entrainment agent pump, carry out cycling extraction again, reach the high efficiente callback of active principle.
The component concentration of table 1 high-ester flavouring liquid
Claims (2)
1. a method of extracting wine high-ester flavouring liquid from wine tail, is characterized in that comprising the steps:
(1) selection of wine tail: selecting wine unstrained spirits fermentation period is the aromatic Chinese spirit fermentation pit of 4 to 6 months, and select the wine unstrained spirits dividing near bottom, Jiao Chi pond, wine unstrained spirits obtains the lower concentration wine tail of alcoholic strength in 15%～20% scope through the distillation of rice steamer bucket;
(2) pre-treatment step of wine tail: by above-mentioned selected low boilers for low-proof wine stratification, collect the floating oily matter in wine tail upper strata, obtain wine tail oily matter;
(3) extraction step: the wine tail oily matter of step 2 is placed in to supercritical CO
2extraction kettle in, regulating extraction kettle pressure is 7.5～8Mpa, extraction kettle temperature is 35～45 DEG C; Extraction time is 1h～2h; Make esters of gallic acid material in wine tail be dissolved in supercritical CO
2in fluid;
(4) separating step: will carry the CO of esters of gallic acid material in step (3)
2fluid successively enters separating still I and separating still II; Described separating still I pressure is 6.5～7Mpa, and separating still I temperature is 35～40 DEG C; Separating still II pressure is 4.5～5Mpa, and separating still II temperature is 25～35 DEG C, by reducing CO in separating still
2pressure, esters of gallic acid material is resolved in separating still; The parsing thing of collecting separating still II, this parsing thing is colourless transparent liquid, is high-ester flavouring liquid.
2. a kind of method of extracting wine high-ester flavouring liquid from wine tail according to claim 1, it is characterized in that, the parsing thing obtaining in separating still I in described step (4) is forwarded in extraction kettle and carries out cycling extraction separation, to reach the high efficiente callback of active principle.
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| CN201210189220.4A CN103146517B (en) | 2012-06-08 | 2012-06-08 | Method for extracting high-ester seasoning liquid from after-run |
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| CN201210189220.4A CN103146517B (en) | 2012-06-08 | 2012-06-08 | Method for extracting high-ester seasoning liquid from after-run |
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| CN103146517B true CN103146517B (en) | 2014-07-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104357299B (en) * | 2014-11-10 | 2016-08-24 | 江苏洋河酒厂股份有限公司 | A kind of production method of peracid ester flavouring wine |
| CN106047577A (en) * | 2016-08-19 | 2016-10-26 | 四川远鸿小角楼酒业有限公司 | Method for producing flavor distilling wine blending liquid by using yellow water |
| CN109198578A (en) * | 2018-11-07 | 2019-01-15 | 广东石湾酒厂集团有限公司 | A method of high concentration esters blending liquor is prepared using soybean-flavor liquor by-product |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU889693A1 (en) * | 1979-06-07 | 1981-12-15 | Всесоюзный Заочный Институт Пищевой Промышленности | Method of producing brandy alcohol |
| CN1970722A (en) * | 2006-11-28 | 2007-05-30 | 李家民 | Supercritical CO2 extraction method for aromatic matter in brewed spirit solid |
| RU2421510C1 (en) * | 2010-05-05 | 2011-06-20 | Общество с ограниченной ответственностью "Научно-внедренческое предприятие "Эффект-91" | Distillate production method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441675C (en) * | 2005-12-30 | 2008-12-10 | 郑州轻工业学院 | Method for Extracting Residual Liquor Aroma Components in Distiller's Grains |
| CN100415866C (en) * | 2006-07-12 | 2008-09-03 | 四川省宜宾五粮液集团有限公司 | Method for extracting flavor and aroma substances for wine from wine tail |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU889693A1 (en) * | 1979-06-07 | 1981-12-15 | Всесоюзный Заочный Институт Пищевой Промышленности | Method of producing brandy alcohol |
| CN1970722A (en) * | 2006-11-28 | 2007-05-30 | 李家民 | Supercritical CO2 extraction method for aromatic matter in brewed spirit solid |
| RU2421510C1 (en) * | 2010-05-05 | 2011-06-20 | Общество с ограниченной ответственностью "Научно-внедренческое предприятие "Эффект-91" | Distillate production method |
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