CN102002428B - Method for extracting volatile oil from geotrichum candidum through fermentation of burdock by utilizing supercritical extraction method and application - Google Patents
Method for extracting volatile oil from geotrichum candidum through fermentation of burdock by utilizing supercritical extraction method and application Download PDFInfo
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- CN102002428B CN102002428B CN2009100637998A CN200910063799A CN102002428B CN 102002428 B CN102002428 B CN 102002428B CN 2009100637998 A CN2009100637998 A CN 2009100637998A CN 200910063799 A CN200910063799 A CN 200910063799A CN 102002428 B CN102002428 B CN 102002428B
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- CN
- China
- Prior art keywords
- volatile oil
- great burdock
- burdock achene
- geotrichum candidum
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Seasonings (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a method for extracting volatile oil from geotrichum candidum through the fermentation of burdock by utilizing a supercritical extraction method and an application, belonging to the technical field of tobacco spice extraction. The method of the invention adopts the geotrichum candidum to ferment and degrade the grease components harmful to the sensory quality of tobacco, carries out the supercritical carbon dioxide extraction to obtain the burdock volatile oil after the fermentation, has the advantages of effective measures and obvious technical effects, and is simple in operation and easy in implementation, and the extracted volatile oil has the advantages of high yield and good quality. The obtained burdock volatile oil contains more fragrant components same or similar to the tobacco, can be coordinated with the initial fragrance of the tobacco when being added to tobacco shreds, and has the effect of enriching and coordinating the tobacco fragrance, promoting the quality of the tobacco fragrance and reducing the simulation. Particularly, the micro-molecular organic acid generated from the grease components after degradation can effectively enhance the tobacco fragrance and reduces the simulation.
Description
Technical field
The invention belongs to cigarette flavors extractive technique field, be specifically a kind of with the plant amedica Great Burdock Achene through after the geotrichum candidum fermentation, adopt supercritical extraction therefrom to extract the method for volatile oil, and the volatile oil that extracts as the application of cigarette additive.
Background technology
In the prior art, Great Burdock Achene, " Pharmacopoeia of People's Republic of China (one one) " (version in 2005) includes, and is the dry mature fruit of feverfew burdock Arctium lappa L..The infructescence of gathering during fruit maturation autumn is dried, and lays fruit.All there is distribution all parts of the country, and the beginning is stated from " Mingyi Bielu ", classifies middle article as.Great Burdock Achene has another name called: dislike reality, FRUCTUS ARCTII, the sticking son of broomcorn millet, Fructus Arctii, bat thorn, Mao Ranran, reshahar is sub, pin feather is sub, sticking grey son, mouse ace, the curved hook, ten thousand that clings to be hook, ox, Niu Zi greatly; Its anaesthetic is called Xi Bai-Wu Busi, Tibetan medicine west by name pine.Proterties: the achene long inverted ovoid, slightly flat, microbend, long 5-7mm, wide 2-3mm.The surface beige, band atropurpureus spot has several vertical ribs, and usually middle 1-2 bar is more obvious.The blunt circle in top, wide slightly, end face has annulus.Middle tool point-like style vestiges; Base portion is slightly narrow, and areola is more shallow.Pericarp is hard, two oyster whites of cotyledon, oil.Odorless, little suffering behind the bitter and numb slightly tongue.Cold in nature, flavor is hot, bitter.Attach to the lung and stomach meridians.Function cures mainly: dispelling wind and heat pathogens, a surname's lung promoting eruption, resolving toxin and disinhibiting the throat.Modern pharmacological research finds that Great Burdock Achene has the function of following several respects: antibiotic, antivirus action; The effect of calcium antagonist appearance; Raise immunity and hypoglycemic activity; Anti-ephrosis becomes; Antitumor, mutation effect; Diuresis and discharge function etc.
The research of Great Burdock Achene and range of application are mainly in pharmaceutical industries in the prior art; As: Chinese patent document CN101134031 discloses the purposes of l-arctigenin in the medicine of preparation treatment or prevention chronic renal failure and renal fibrosis; Its extract is mainly l-arctigenin, is used for ephrosis.Chinese patent document CN1560265 discloses a kind of method for preparing antiviral and antitumor natural drug l-arctigenin; Extract is the pure article of l-arctigenin, is used for antiviral, antitumor.Chinese patent document CN1569138 discloses a kind of preparation method with Fructus Arctii extract of hypoglycemic activity, and extract mainly is arctinin, l-arctigenin and mataires inal, is used for hypoglycemic.Chinese patent document CN1879644 discloses the purposes of arctinin aspect the preparation anti-inflammatory drug, and extract is an arctinin, is used for anti-inflammatory.From prior art; We know the 5-10% that the arctinin that contained in the Great Burdock Achene medicinal material and l-arctigenin are about the medicinal material total amount; Still there is other a large amount of materials not to be employed in the Great Burdock Achene medicinal material, all is not used effectively like materials such as volatile oil, carbohydrate, amino acids, alkaloidss.And relevant report is not also seen in the application of Great Burdock Achene in cigarette, does not see to have to prepare the relevant report of cigarette with the method for Fructus Arctii extract yet.
The chemical ingredients of Great Burdock Achene mainly contains: volatile oil, oils, Arctiin (Arctiin), aretigenin (Arctigenin), burdock phenols, polyose, amino acids, alkaloids, sterols, vitamins etc.Volatile oil content is generally about 0.1～1% in the Great Burdock Achene.In volatile oil component, pulegone content is the highest, accounts for 25% of volatile oil component total amount; Other also comprises some terpenes, micromolecular aldoketones and aldehydes matter, and these materials have strong fragrance, is the fragrant material of increase cigarette that often uses in the cigarette blending; Therefore, utilize the volatile oil material in the Great Burdock Achene, be used for cigarette flavors; Increasing cigarette flavor is a kind of feasible technological development direction, and, there is not the people to carry out a large amount of work as yet in this field.
In the prior art, the most popular method of the extraction burdock seed oil that pharmaceutical industries adopts is wet distillation and supercritical carbon dioxide extraction.But, containing 26～30% the oils composition of having an appointment in the Great Burdock Achene, content is very high, comprises palmitic acid, stearic acid, oleic acid, linolic acid, linolenic acid etc.The method that prior art is directly extracted volatile oil makes and contains more above-mentioned oil substances in the extract.And these oils compositions add in the cigarette, can bring more serious assorted gas, stimulation and oral cavity residual, influence the cigarette quality.
Document [Luo Yongming, Zhu Ying, Li Bin etc., the GC-MS of Great Burdock Achene volatile oil component analyzes, Chinese medicinal materials, 1997,20 (12): 621-623] adopt the method for wet distillation to obtain Great Burdock Achene volatile oil the Great Burdock Achene medicinal material coarse powder.But the method for wet distillation has following defective: 1, wet distillation is owing to be pyrogenic distillation, the structure of some heat-sensitive substances changed or component reacts each other, thereby changed the structure and the composition of natural constituents.2, wet distillation is consuming time longer, and energy consumption is bigger.3, wet distillation mode Great Burdock Achene volatile oil yield is lower, is about 0.2%.
Supercritical carbon dioxide fluid is made solvent and is extracted; Characteristics with the protection of low-temperature extraction and inertia have prevented contingent reacting to each other between oxidation and the loss and the different components of " susceptibility " material, make extraction be easy to unite two into one with separating; Production efficiency and energy efficient have been improved effectively; Can exempt any poisonous and hazardous organic solvent fully in process of production, extract does not contain organic dissolvent residual, has kept the All Pure Nature property of extract.Whole process does not produce " three wastes ", can not pollute environment.But document [Liu Renmin, Zhang Kun, Cui Qingxin.The supercritical carbon dioxide extraction research of burdock seed oil; Teachers college, Liaocheng journal (natural science edition), 2002,15 (4): 32-35] prove; Adopt supercritical carbon dioxide fluid directly to extract the Great Burdock Achene medicinal material coarse powder and obtain the burdock seed oil, what extract mainly is the oils composition.As stated, these compositions all are not suitable for directly applying to cigarette.
Geotrichum candidum (Geotrichum candidum), Deuteromycotina, hyphomycetes, hyphomycetales, Moniliaceae, Geotrichum, fungi a kind of.Mycelia is the fungal filament that tabula is arranged, and what have is dichotomy.Wide 3～7 μ m of mycelia.Fragment into the arthrospore of single or chaining, long tubular, terminal blunt circle after the mycelia maturation.The arthrospore size is (4.9～7.6 μ m) * (5.4～16.6 μ m).Bacterium colony is planar diffusion, and growth is fast, and is flat, oyster white, and short flannel shape or be bordering on powdery, but the concentric turns radioactive rays are arranged, what have is umbo.Effective type of cutting grease material.
Summary of the invention
Above-mentioned deficiency to prior art; The technical problem that the present invention will solve provides a kind of method of geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil; It can both remove the disadvantageous oil substances to the cigarette aesthetic quality; Can keep the volatile oil material favourable again, utilize the various beneficiating ingredients in the natural drug Great Burdock Achene fully the cigarette aesthetic quality.The volatile oil that is extracted is applied to tobacco, can play the effect that improves the tobacco product quality.
Technical scheme of the present invention is: the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil reaches condition according to the following steps and carries out:
[1], the Chinese medicinal materials Great Burdock Achene was ground into the meal of 100 mesh sieves, with nutritive medium by 20～50: after 1 mass ratio mixes, in 115 ℃ of sterilization 15～20min down;
[2], the activated seed liquid of fungi geotrichum candidum bacterial classification is inoculated in the aseptic Great Burdock Achene meal according to 1: 10～50 mass ratio; Stir; Make meal solid and seed liquor thorough mixing even, the Great Burdock Achene meal of having inoculated fungi geotrichum candidum bacterial classification is positioned in 25～30 ℃ the incubator and fermented 2～7 days;
[3], the Great Burdock Achene meal after will fermenting adds in the supercritical extraction reactor and carries out supercritical extraction; Extraction conditions is: the extraction temperature of CO 2 fluid is 45～55 ℃; Pressure is 25～40MPa, the flow 30～90kg/h of carbonic acid gas, entrainment agent flow 30～60kg/h in the auxiliary pump; The separation temperature of separating still is 35～50 ℃, and pressure is 8～10MPa; The extraction time is 60～120min; The light yellow oily extract of gained is a Great Burdock Achene volatile oil.
Described entrainment agent is 95% edible ethanol, and the amount of entrainment agent is 3-6 a times of Great Burdock Achene meal weight.
Described separating still is one or more.
The activated seed liquid of described fungi geotrichum candidum bacterial classification reaches condition according to the following steps and handles: get the fungi geotrichum candidum bacterial classification that preserve in the laboratory, be inoculated on the slant medium, be positioned in 25～30 ℃ the constant incubator and cultivate 24～48h; Be inoculated in the liquid nutrient medium that adds sugared source; In 25～30 ℃ of constant temperature culture 24～48h, seed liquor is centrifugal, abandon supernatant; The deposition thalline with saline water dilution concussion evenly obtains the activatory seed liquor.
The liquid nutrient medium in the sugared source of described interpolation is the mixed solution of following material: K
2HPO
41g, MgSO
47H
2O 0.5g, peptone 5g, glucose 10g, water 1000mL.
Described nutritive medium is the mixed solution of following material: peptone 1g, glucose 2g, NaCl 0.05g, K
2HPO
40.01g, MgSO
47H
2O 0.05g, water 1000mL.
The application of a kind of geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil: Great Burdock Achene volatile oil is become 1% with 95% alcohol dilution, add in the pipe tobacco according to 0.01～0.05% of pipe tobacco weight then.
Advantage of the present invention:
Adopt the geotrichum candidum fermentation energy effectively to degrade to the disadvantageous oils composition of cigarette aesthetic quality; Generation increases cigarette ageing acid perfume and the small molecular organic acid constituents that reduces hormesis to favourable the having of cigarette aesthetic quality; Unfavorable composition is converted into favourable composition, has promoted the quality of Great Burdock Achene volatile oil as cigaret additive.Carrying out the effect of Great Burdock Achene volatile oil in cigarette that supercritical carbon dioxide extraction obtains after the fermentation again is better than nonfermented greatly and directly carries out the Great Burdock Achene volatile oil that supercritical carbon dioxide extraction obtains.
Adopt the supercritical carbon dioxide extraction mode; Characteristics with the protection of low-temperature extraction and inertia have prevented contingent reacting to each other between oxidation and the loss and the different components of " susceptibility " material, make extraction be easy to unite two into one with separating; Production efficiency and energy efficient have been improved effectively; Can exempt any poisonous and hazardous organic solvent fully in process of production, extract does not contain organic dissolvent residual, has kept the All Pure Nature property of extract.Whole process does not produce " three wastes ", can not pollute environment.
Adopt the Great Burdock Achene after supercritical carbon dioxide extraction ferments, the yield of volatile oil is 2.95%, and the wet distillation yield is 0.20%, and method of the present invention is superior to the method for prior art greatly.
A lot of identical or similar flavour ingredients of flavour ingredient that contain with tobacco itself are arranged in the Great Burdock Achene volatile oil that the present invention obtains, add in the pipe tobacco and can coordinate with this perfume of tobacco, have abundant and coordination cigarette perfume, lifting tobacco aroma matter reduces the effect that stimulates.Especially the small molecular organic acid that generates after the degraded of oils composition can effectively increase cigarette perfume and reduce stimulation.
Embodiment
Below in conjunction with embodiments of the invention the relevant technologies problem is described in further detail.
Embodiment 1 gets the fungi geotrichum candidum bacterial classification that preserve in the laboratory, is inoculated on the slant medium, is positioned in 30 ℃ the constant incubator and cultivates 24h, is inoculated in the liquid nutrient medium (K that adds sugared source
2HPO
41g, MgSO
47H
2O 0.5g, peptone 5g, glucose 10g, water 1000mL) in, in 30 ℃ of constant temperature culture 24h, with the centrifugal supernatant of abandoning of seed liquor, the deposition thalline with saline water dilution concussion evenly obtains the activatory seed liquor.
The Chinese medicinal materials Great Burdock Achene was ground into the meal of 100 mesh sieves, with nutritive medium (peptone 1g, glucose 2g, NaCl 0.05g, K
2HPO
40.01g, MgSO
47H
2O 0.05g, water 1000mL) mix by 20: 1 mass ratioes after, in 115 ℃ of sterilization 15min down.
The mass ratio of the seed liquor of handling well according to 1: 10 is inoculated in the aseptic Great Burdock Achene meal, stirs, make meal solid and seed liquor thorough mixing even, the Great Burdock Achene meal that inoculation is good is positioned in 30 ℃ the incubator and fermented 2 days.
With carrying out supercritical extraction in the adding of the Great Burdock Achene meal after the fermentation supercritical extraction reactor; Extraction conditions is that the extraction temperature of CO 2 fluid is 45 ℃; Pressure is 25MPa, the flow 30kg/h of carbonic acid gas, entrainment agent 95% edible ethanol flow 30kg/h in the auxiliary pump; The separation temperature of separating still is 35 ℃, and pressure is 8MPa; The extraction time is 60min.The light yellow oily extract of gained is a Great Burdock Achene volatile oil.
Great Burdock Achene volatile oil is become 1% solution with 95% alcohol dilution, add in the high-grade cigarette pipe tobacco according to 0.01% of pipe tobacco weight then, smoke panel test according to national standard method after making cigarette.Smoking result is: the ageing acid that increases cigarette is fragrant, the rich obvious increase that cigarette is fragrant, and have the effect that tangible reduction stimulates.
Embodiment 2 gets the fungi geotrichum candidum bacterial classification that preserve in the laboratory, is inoculated on the slant medium, is positioned in 28 ℃ the constant incubator and cultivates 36h, is inoculated in the liquid nutrient medium (K that adds sugared source
2HPO
41g, MgSO
47H
2O 0.5g, peptone 5g, glucose 10g, water 1000mL) in, in 28 ℃ of constant temperature culture 36h, with the centrifugal supernatant of abandoning of seed liquor, the deposition thalline with saline water dilution concussion evenly obtains the activatory seed liquor.
The Chinese medicinal materials Great Burdock Achene was ground into the meal of 100 mesh sieves, with nutritive medium (peptone 1g, glucose 2g, NaCl 0.05g, K
2HPO
40.01g, MgSO
47H
2O 0.05g, water 1000mL) mix by 30: 1 mass ratioes after, in 115 ℃ of sterilization 20min down.
The mass ratio of the seed liquor of handling well according to 1: 25 is inoculated in the aseptic Great Burdock Achene meal, stirs, make meal solid and seed liquor thorough mixing even, the Great Burdock Achene meal that inoculation is good is positioned in 28 ℃ the incubator and fermented 5 days.
With carrying out supercritical extraction in the adding of the Great Burdock Achene meal after the fermentation supercritical extraction reactor; Extraction conditions is that the extraction temperature of CO 2 fluid is 50 ℃; Pressure is 35MPa, the flow 60kg/h of carbonic acid gas, entrainment agent 95% edible ethanol flow 45kg/h in the auxiliary pump; The separation temperature of separating still is 45 ℃, and pressure is 8MPa; The extraction time is 60min.The light yellow oily extract of gained is a Great Burdock Achene volatile oil.
Great Burdock Achene volatile oil is become 1% solution with 95% alcohol dilution, add in the middle-grade shelves cigarette shreds according to 0.02% of pipe tobacco weight then, smoke panel test according to national standard method after making cigarette.Smoking result is: the ageing acid that increases cigarette is fragrant, increases flue gas concentration, and has the effect that tangible reduction stimulates.
Embodiment 3 gets the fungi geotrichum candidum bacterial classification that preserve in the laboratory, is inoculated on the slant medium, is positioned in 25 ℃ the constant incubator and cultivates 48h, is inoculated in the liquid nutrient medium (K that adds sugared source
2HPO
41g, MgSO
47H
2O 0.5g, peptone 5g, glucose 10g, water 1000mL) in, in 25 ℃ of constant temperature culture 48h, with the centrifugal supernatant of abandoning of seed liquor, the deposition thalline with saline water dilution concussion evenly obtains the activatory seed liquor.
The Chinese medicinal materials Great Burdock Achene was ground into the meal of 100 mesh sieves, with nutritive medium (peptone 1g, glucose 2g, NaCl 0.05g, K
2HPO
40.01g, MgSO
47H
2O 0.05g, water 1000mL) mix by 50: 1 mass ratioes after, in 115 ℃ of sterilization 20min down.
The mass ratio of the seed liquor of handling well according to 1: 50 is inoculated in the aseptic Great Burdock Achene meal, stirs, make meal solid and seed liquor thorough mixing even, the Great Burdock Achene meal that inoculation is good is positioned in 25 ℃ the incubator and fermented 7 days.With carrying out supercritical extraction in the adding of the Great Burdock Achene meal after the fermentation supercritical extraction reactor; Extraction conditions is that the extraction temperature of CO 2 fluid is 55 ℃; Pressure is 40MPa, the flow 90kg/h of carbonic acid gas, entrainment agent 95% edible ethanol flow 60kg/h in the auxiliary pump; The separation temperature of separating still is 50 ℃, and pressure is 10MPa; The extraction time is 120min.The light yellow oily extract of gained is a Great Burdock Achene volatile oil.
Great Burdock Achene volatile oil is become 1% solution with 95% alcohol dilution, add in the Low-end Cigarettes pipe tobacco according to 0.05% of pipe tobacco weight then, smoke panel test according to national standard method after making cigarette.Smoking result is: the ageing acid that increases cigarette is fragrant, covers the assorted gas of Low-end Cigarettes, and has the effect that tangible reduction stimulates.
Study through the applicant; Recognize that unemployed these compositions in the Great Burdock Achene medicinal material all have better action to the aesthetic quality of tobacco: wherein; The volatile oil material: wherein pulegone content is the highest, accounts for 25% of volatile oil component total amount, and other also comprises some terpenes, micromolecular aldoketones and aldehydes matter; These materials have strong fragrance, are the fragrant materials of increase cigarette that often uses in the cigarette blending.
The applicant recognizes effectively type of the cutting grease Substance Properties that geotrichum candidum has; Therefore; Consider to adopt geotrichum candidum that Great Burdock Achene is fermented in advance; Effective degraded generates cigarette sense organ favourable having increasing cigarette ageing acid perfume and the small molecular organic acid constituents that reduces hormesis the disadvantageous oils composition of cigarette sense organ, and unfavorable composition is converted into favourable composition.
The contriver has carried out the composition evaluation with the gas chromatography appearance to Great Burdock Achene volatile oil, and condition determination is following:
Instrument is a Thermo TRACE GC Ultra-DSQ II makings logotype appearance.GC conditions: chromatographic column DB-5ms 30 * 0.25mm * 0.25 μ m; 50 ℃ of initial column temperatures keep 1min, with 10 ℃/min temperature programming to 250 ℃, keep temperature 10min then; 250 ℃ of injector temperatures; Carrier gas He, flow velocity 1.0ml/min; Sample size 0.5 μ l, splitting ratio 100: 1.MS condition: EI ion source, electron energy 70eV, sweep limit 35～650amu, 220 ℃ of ion source temperatures, Multiplier voltage 1500V, 250 ℃ GC/MS interfaces, spectrum storehouse NIST98.The area normalization method is quantitative.
Volatile oil and Great Burdock Achene volatile oil of the present invention that the Great Burdock Achene volatile oil that the applicant obtains wet distillation, direct supercritical extraction obtain have carried out GC/MS composition analysis contrast, and the result sees table 1.
Table 1 Great Burdock Achene volatile oil component and relative content synopsis
| The composition title | Each composition relative content (%) of the volatile oil that wet distillation obtains | Each composition relative content (%) of volatile oil that direct supercritical extraction obtains | Each composition relative content (%) of the volatile oil that the present invention obtains |
| The 2-methylcyclopentanol | 3.29 | Do not detect | 1.35 |
| Isopropylformic acid | Do not detect | Do not detect | 5.98 |
| Butyric acid | 0.56 | Do not detect | 41.44 |
| Isovaleric acid | Do not detect | Do not detect | 3.43 |
| 3-methyl-butyric acid | Do not detect | Do not detect | 2.36 |
| Valeric acid | Do not detect | Do not detect | 3.17 |
| 2-heptanone | 2.74 | Do not detect | 1.15 |
| 2 methyl cyclohexanol | 0.42 | Do not detect | 0.41 |
| 4,5-dimethyl--tetrahydrobenzene-1-ketone | 0.32 | Do not detect | 0.39 |
| 4 methyl cyclohexanol | 0.86 | Do not detect | 0.42 |
| Caproic acid | Do not detect | Do not detect | 2.61 |
| Methyl phenyl ketone | 0.54 | Do not detect | 1.14 |
| 1-teracrylic acid-alcohol | 3.22 | Do not detect | 1.32 |
| 2-amyl furan | 1.36 | Do not detect | 0.62 |
| Enanthic acid | 0.66 | Do not detect | 3.21 |
| Phenyl aldehyde | 0.69 | Do not detect | 0.47 |
| Therapeutic Mineral Ice | 0.78 | Do not detect | 0.49 |
| Phenylethyl alcohol | 0.17 | Do not detect | 0.86 |
| Cyclononanone | 0.47 | Do not detect | 0.77 |
| Lindenol | 0.24 | Do not detect | 0.68 |
| Phenylformic acid | Do not detect | Do not detect | 2.84 |
| Methyl Salicylate | 0.42 | Do not detect | 0.26 |
| Homoanisic acid | 0.38 | Do not detect | 0.35 |
| The O-methoxy toluylic acid | 0.32 | Do not detect | 0.26 |
| Toluylic acid | Do not detect | Do not detect | 1.76 |
| 2-methyl-5-pseudoallyl pimelinketone | 0.78 | Do not detect | 0.46 |
| Pulegone | 24.67 | Do not detect | 9.62 |
| 3-methyl-6-propylphenol | 5.36 | Do not detect | 0..75 |
| Carvotanacetone | 2.82 | Do not detect | 0.44 |
| P-methoxy phenyl acetone | 3.44 | Do not detect | 0.65 |
| 4-hydroxy 3-methoxybenzene formaldehyde | 1.69 | Do not detect | 0.42 |
| γ-Elemenum | 0.37 | Do not detect | 0.28 |
| Chamene | 0.35 | Do not detect | 0.22 |
| γ-cadinene | 0.21 | Do not detect | 0.18 |
| 4-hydroxy 3-methoxybenzene ethyl ketone | 3.63 | Do not detect | 0.64 |
| 3, the 4-dimethoxy benzaldehyde | 4.23 | Do not detect | 0.43 |
| Cypress camphor | 3.76 | Do not detect | 0.95 |
| β-eucalyptus alcohol | 4.48 | Do not detect | 0.98 |
| Palmitic acid | 1.14 | 9.87 | 0.15 |
| Linolic acid | 5.68 | 52.34 | 0.43 |
| Oleic acid | 2.73 | 24.61 | 0.26 |
| Stearic acid | 0.45 | 3.54 | 0.07 |
| Linolenic acid | 0.21 | 1.27 | Do not detect |
Through contrast, can find out that directly carrying out the volatile oil staple that supercritical extraction obtains is exactly oil substances.Volatile oil that the present invention's extraction obtains and wet distillation are relatively; Have increase cigarette ageing acid fragrant with the small molecular organic acid that reduces hormesis as: butyric acid, isopropylformic acid, 3 Methylbutanoic acid, valeric acid, isovaleric acid, caproic acid, phenylformic acid, toluylic acid all are not have in the wet distillation product; Obtain through the oils degraded; Account for 63.59% of volatile oil component that the present invention obtains, especially butyric acid content accounts for 41.44%.Because the generation of a large amount of small molecular organic acids improves the yield of volatile oil greatly, so the relative content of pulegone reduces.And palmitic acid, stearic acid etc. can bring more serious assorted gas, stimulation and oral cavity residual, and the fatty acid component content that influences the cigarette quality obviously reduces.Therefore, the volatile oil that obtains of the present invention extraction in cigarette flavoring, increase cigarette ageing acid fragrant with reduce the effect that stimulates can be better.
The Great Burdock Achene volatile oil that the applicant obtains wet distillation, the directly Great Burdock Achene volatile oil that obtains of supercritical extraction and the Great Burdock Achene volatile oil of the present invention contrast of smokeing panel test; Smoke panel test and carry out according to national standard method; 7 people form the group of smokeing panel test; 2 national judging panels, 5 provincial judging panels, smoking result such as following table 2.Visible from table, Great Burdock Achene volatile oil of the present invention, apply with pipe tobacco after, the aesthetic quality that can improve cigarette.
Table 2 contrast table of smokeing panel test
| The Great Burdock Achene volatile oil that wet distillation obtains | Fragrance passes through and sends out, and the flue gas exquisiteness is soft, concentration increases, and tongue slightly stagnates. |
| The Great Burdock Achene volatile oil that direct supercritical extraction obtains | Concentration increases, and stimulates to increase, and assorted gas is heavier, and lingual surface is residual heavier. |
| Great Burdock Achene volatile oil of the present invention | The ageing acid that increases cigarette is fragrant, and obviously reducing stimulates, and does not have obviously residual. |
Claims (7)
1. the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil is characterized in that described method reaches condition according to the following steps and carries out:
[1], the Chinese medicinal materials Great Burdock Achene was ground into the meal of 100 mesh sieves, with nutritive medium by 20～50: after 1 mass ratio mixes, in 115 ℃ of sterilization 15～20min down;
[2], the activated seed liquid of fungi geotrichum candidum bacterial classification is inoculated in the aseptic Great Burdock Achene meal according to 1: 10～50 mass ratio; Stir; Make meal solid and seed liquor thorough mixing even, the Great Burdock Achene meal of having inoculated fungi geotrichum candidum bacterial classification is positioned in 25～30 ℃ the incubator and fermented 2～7 days;
[3], the Great Burdock Achene meal after will fermenting adds in the supercritical extraction reactor and carries out supercritical extraction; Extraction conditions is: the extraction temperature of CO 2 fluid is 45～55 ℃; Pressure is 25～40MPa, the flow 30～90kg/h of carbonic acid gas, entrainment agent flow 30～60kg/h in the auxiliary pump; The separation temperature of separating still is 35～50 ℃, and pressure is 8～10MPa; The extraction time is 60～120min; The light yellow oily extract of gained is a Great Burdock Achene volatile oil.
2. the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil according to claim 1, it is characterized in that: described entrainment agent is 95% edible ethanol, the amount of entrainment agent is 3-6 a times of Great Burdock Achene meal weight.
3. the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil according to claim 1, it is characterized in that: described separating still is one or more.
4. the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil according to claim 1; It is characterized in that: the activated seed liquid of described fungi geotrichum candidum bacterial classification reaches condition according to the following steps and handles: get the fungi geotrichum candidum bacterial classification that preserve in the laboratory, be inoculated on the slant medium, be positioned in 25～30 ℃ the constant incubator and cultivate 24～48h; Be inoculated in the liquid nutrient medium that adds sugared source; In 25～30 ℃ of constant temperature culture 24～48h, seed liquor is centrifugal, abandon supernatant; The deposition thalline is even with saline water dilution concussion, and gained is the activatory seed liquor.
5. the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil according to claim 4, it is characterized in that: the liquid nutrient medium in the sugared source of described interpolation is the mixed solution of following material: K
2HPO
41g, MgSO
47H
2O 0.5g, peptone 5g, glucose 10g, water 1000mL.
6. the method for geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil according to claim 1, it is characterized in that: described nutritive medium is the mixed solution of following material: peptone 1g, glucose 2g, NaCl 0.05g, K
2HPO
40.01g, MgSO
47H
2O 0.05g, water 1000mL.
7. the application of the Great Burdock Achene volatile oil that obtains of geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction is characterized in that: Great Burdock Achene volatile oil is become 1% with 95% alcohol dilution, add in the pipe tobacco according to 0.01～0.05% of pipe tobacco weight then.
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| CN104126868B (en) * | 2014-07-18 | 2016-08-24 | 云南中烟工业有限责任公司 | Come from the preparation method of the natural perfume material of bolete and to the purposes of fragrance-enhancing tobacco |
| CN104804874A (en) * | 2015-04-22 | 2015-07-29 | 湖北中烟工业有限责任公司 | Method for extracting caffeol with supercritical carbon dioxide and application of method for cigarettes |
| CN106280684A (en) * | 2016-08-17 | 2017-01-04 | 张静 | A kind of preparation method of environmental-friendly plant oil-based ink binder |
| CN106433989B (en) * | 2016-11-12 | 2019-11-12 | 郑州雪麦龙食品香料有限公司 | A kind of method of many fragrant fruit oil of subcritical normal butane fluid extraction |
| CN108998232A (en) * | 2018-09-11 | 2018-12-14 | 韩城市宏达花椒香料有限公司 | A kind of preparation method of ziran oil |
| CN109536268B (en) * | 2018-12-21 | 2020-05-08 | 江南大学 | Method for preparing functional grease through segmented solid-state fermentation of mixed fungi |
| CN115363236B (en) * | 2022-08-29 | 2023-04-21 | 湖北中烟工业有限责任公司 | Preparation method of tobacco flavor with sour flavor and sweet flavor and application of tobacco flavor |
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| CN101497844A (en) * | 2008-01-30 | 2009-08-05 | 湖北中烟工业有限责任公司 | Method for preparing cigarette flavor by microbial fermentation of coffee |
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| CN101497844A (en) * | 2008-01-30 | 2009-08-05 | 湖北中烟工业有限责任公司 | Method for preparing cigarette flavor by microbial fermentation of coffee |
| CN101496637A (en) * | 2008-01-30 | 2009-08-05 | 湖北中烟工业有限责任公司 | Method for extracting additive agent for tobacco from common hogfennel root with supercritical extraction |
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