CN102002428A - 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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- CN102002428A CN102002428A CN2009100637998A CN200910063799A CN102002428A CN 102002428 A CN102002428 A CN 102002428A CN 2009100637998 A CN2009100637998 A CN 2009100637998A CN 200910063799 A CN200910063799 A CN 200910063799A CN 102002428 A CN102002428 A CN 102002428A
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- China
- Prior art keywords
- volatile oil
- great burdock
- burdock achene
- geotrichum candidum
- extraction
- Prior art date
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- Granted
Links
- 235000003130 Arctium lappa Nutrition 0.000 title claims abstract description 87
- 239000000341 volatile oil Substances 0.000 title claims abstract description 64
- 244000168141 Geotrichum candidum Species 0.000 title claims abstract description 31
- 235000017388 Geotrichum candidum Nutrition 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 28
- 238000000855 fermentation Methods 0.000 title claims abstract description 20
- 230000004151 fermentation Effects 0.000 title claims abstract description 20
- 240000005528 Arctium lappa Species 0.000 title claims description 85
- 235000008078 Arctium minus Nutrition 0.000 title abstract description 8
- 241000208125 Nicotiana Species 0.000 claims abstract description 24
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims description 28
- 235000012054 meals Nutrition 0.000 claims description 27
- 239000000284 extract Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 241000233866 Fungi Species 0.000 claims description 12
- 230000001580 bacterial effect Effects 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 10
- 239000001888 Peptone Substances 0.000 claims description 10
- 108010080698 Peptones Proteins 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000010790 dilution Methods 0.000 claims description 10
- 239000012895 dilution Substances 0.000 claims description 10
- 239000008103 glucose Substances 0.000 claims description 10
- 235000019319 peptone Nutrition 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 235000015097 nutrients Nutrition 0.000 claims description 7
- 230000000050 nutritive effect Effects 0.000 claims description 7
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 claims description 5
- 235000011089 carbon dioxide Nutrition 0.000 claims description 5
- 230000009514 concussion Effects 0.000 claims description 5
- 239000002504 physiological saline solution Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 230000001954 sterilising effect Effects 0.000 claims description 5
- 238000004659 sterilization and disinfection Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 11
- 239000003205 fragrance Substances 0.000 abstract description 7
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 abstract description 7
- 150000007524 organic acids Chemical class 0.000 abstract description 6
- 235000013599 spices Nutrition 0.000 abstract description 5
- 239000004519 grease Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
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- 238000004088 simulation Methods 0.000 abstract 2
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- 238000006731 degradation reaction Methods 0.000 abstract 1
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- 235000019504 cigarettes Nutrition 0.000 description 41
- 239000000203 mixture Substances 0.000 description 18
- 238000004821 distillation Methods 0.000 description 13
- 239000002253 acid Substances 0.000 description 9
- 230000032683 aging Effects 0.000 description 8
- 150000002632 lipids Chemical class 0.000 description 8
- 239000002304 perfume Substances 0.000 description 8
- NQWVSMVXKMHKTF-UHFFFAOYSA-N arctigenin Chemical compound C1=C(OC)C(OC)=CC=C1CC1C(CC=2C=C(OC)C(O)=CC=2)C(=O)OC1 NQWVSMVXKMHKTF-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- XOJVHLIYNSOZOO-SWOBOCGESA-N Arctiin Chemical compound C1=C(OC)C(OC)=CC=C1C[C@@H]1[C@@H](CC=2C=C(OC)C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)=CC=2)C(=O)OC1 XOJVHLIYNSOZOO-SWOBOCGESA-N 0.000 description 6
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- 230000002349 favourable effect Effects 0.000 description 5
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- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
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- 230000000391 smoking effect Effects 0.000 description 4
- 238000010561 standard procedure Methods 0.000 description 4
- NZGWDASTMWDZIW-MRVPVSSYSA-N (+)-pulegone Chemical compound C[C@@H]1CCC(=C(C)C)C(=O)C1 NZGWDASTMWDZIW-MRVPVSSYSA-N 0.000 description 3
- NZGWDASTMWDZIW-UHFFFAOYSA-N Pulegone Natural products CC1CCC(=C(C)C)C(=O)C1 NZGWDASTMWDZIW-UHFFFAOYSA-N 0.000 description 3
- USMNOWBWPHYOEA-UHFFFAOYSA-N alpha-thujone Natural products CC1C(=O)CC2(C(C)C)C1C2 USMNOWBWPHYOEA-UHFFFAOYSA-N 0.000 description 3
- 230000000259 anti-tumor effect Effects 0.000 description 3
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- 238000011081 inoculation Methods 0.000 description 3
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 3
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- 239000000243 solution Substances 0.000 description 3
- 230000000638 stimulation Effects 0.000 description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 description 3
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 241000237502 Ostreidae Species 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
- BPYGTFFYYOWDBC-LOVSFRALSA-N arctiin Natural products COc1ccc(C[C@H]2COC(=O)[C@@H]2Cc3ccc(O[C@@H]4O[C@H](C)[C@@H](O)[C@H](O)[C@H]4O)c(OC)c3)cc1OC BPYGTFFYYOWDBC-LOVSFRALSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 231100001261 hazardous Toxicity 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000020636 oyster Nutrition 0.000 description 2
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- 239000000843 powder Substances 0.000 description 2
- 210000000697 sensory organ Anatomy 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 150000003505 terpenes Chemical class 0.000 description 2
- 235000007586 terpenes Nutrition 0.000 description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- NQWVSMVXKMHKTF-JKSUJKDBSA-N (-)-Arctigenin Chemical compound C1=C(OC)C(OC)=CC=C1C[C@@H]1[C@@H](CC=2C=C(OC)C(O)=CC=2)C(=O)OC1 NQWVSMVXKMHKTF-JKSUJKDBSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- YYGRXNOXOVZIKE-UHFFFAOYSA-N Arctigenin Natural products COC1CCC(CC2COC(=O)C2CC3CCC(O)C(C3)OC)CC1OC YYGRXNOXOVZIKE-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229940127291 Calcium channel antagonist Drugs 0.000 description 1
- 235000008495 Chrysanthemum leucanthemum Nutrition 0.000 description 1
- 244000192528 Chrysanthemum parthenium Species 0.000 description 1
- 235000000604 Chrysanthemum parthenium Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000159512 Geotrichum Species 0.000 description 1
- OIFFJDGSLVHPCW-UHFFFAOYSA-N Guayarol Natural products COc1ccc(CC2C(Cc3ccc(O)c(O)c3)COC2=O)cc1OC OIFFJDGSLVHPCW-UHFFFAOYSA-N 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 101100054520 Mus musculus Ace gene Proteins 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000007199 Panicum miliaceum Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 230000003444 anaesthetic effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 229940124599 anti-inflammatory drug Drugs 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 210000004883 areola Anatomy 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 244000022185 broomcorn panic Species 0.000 description 1
- 239000000480 calcium channel blocker Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 208000020832 chronic kidney disease Diseases 0.000 description 1
- 208000022831 chronic renal failure syndrome Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 229930195729 fatty acid Natural products 0.000 description 1
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- 150000004665 fatty acids Chemical class 0.000 description 1
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- 235000008384 feverfew Nutrition 0.000 description 1
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- 230000036039 immunity Effects 0.000 description 1
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 229960004232 linoleic acid Drugs 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- NWFYESYCEQICQP-UHFFFAOYSA-N methylmatairesinol Natural products C1=C(OC)C(OC)=CC=C1CC1C(=O)OCC1CC1=CC=C(O)C(OC)=C1 NWFYESYCEQICQP-UHFFFAOYSA-N 0.000 description 1
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- 238000010606 normalization Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229960002969 oleic acid Drugs 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 229940098695 palmitic acid Drugs 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- -1 polyose Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
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- 230000002285 radioactive effect Effects 0.000 description 1
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- 150000003432 sterols Chemical class 0.000 description 1
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Classifications
-
- 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
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Seasonings (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 product 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, pin feather, sticking grey son, mouse ace, curved crust hook, ten thousand hook, big ox, Niu Zi; 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 sample; 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 literature 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 literature CN1560265 discloses a kind of method for preparing antiviral and antitumor natural drug l-arctigenin; Extract is the pure product of l-arctigenin, is used for antiviral, antitumor.Chinese patent literature 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 literature 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 as materials such as volatile oil, carbohydrate, amino acids, alkaloidss.And the application of Great Burdock Achene in cigarette yet there are no relevant report, also do not see to have to prepare the relevant report of cigarette with the method for Fructus Arctii extract.
The chemical ingredients of Great Burdock Achene mainly contains: volatile oil, lipid, 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, and other also comprises some terpenes, micromolecular aldoketones and aldehydes matter, these materials have strong fragrance, be the material of the frequent increase cigarette perfume (or spice) that 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 lipid 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 lipid 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; prevented contingent reacting to each other between the oxidation of " susceptibility " material and loss and the different components; 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 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 lipid composition.As mentioned above, 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.The class material can effectively cut grease.
Summary of the invention
Above-mentioned deficiency at prior art, the technical problem to be solved in the present invention 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 liquor, the precipitation thalline with physiological saline 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 lipid composition of cigarette aesthetic quality, generation increases cigarette ageing acid perfume to favourable the having of cigarette aesthetic quality and reduces the small molecular organic acid constituents of hormesis, 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; prevented contingent reacting to each other between the oxidation of " susceptibility " material and loss and the different components; 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 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 better than 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, have abundant and coordination cigarette perfume (or spice), promote tobacco aroma matter, the effect that reduction stimulates with this perfume of tobacco.Especially the small molecular organic acid that generates after the degraded of lipid 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 liquor of abandoning of seed liquor, the precipitation thalline with physiological saline 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 seed liquor handled well the mass ratio 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.
To carry 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 of cigarette perfume (or spice), 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 liquor of abandoning of seed liquor, the precipitation thalline with physiological saline 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 seed liquor handled well the mass ratio 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.
To carry 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 liquor of abandoning of seed liquor, the precipitation thalline with physiological saline 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 seed liquor handled well the mass ratio 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.To carry 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, account for 25% of volatile oil component total amount, other also comprises some terpenes, micromolecular aldoketones and aldehydes matter, these materials have strong fragrance, are the materials of the frequent increase cigarette perfume (or spice) that uses in the cigarette blending.
The applicant recognizes the class Substance Properties that effectively cuts grease that geotrichum candidum has, therefore, consider to adopt geotrichum candidum that Great Burdock Achene is fermented in advance, effectively degraded is to the disadvantageous lipid composition of cigarette sense organ, generation is converted into favourable composition to the small molecular organic acid constituents of cigarette sense organ favourable having increasing cigarette ageing acid perfume and reduction hormesis with unfavorable composition.
The contriver has carried out the composition evaluation with the gas chromatography instrument to Great Burdock Achene volatile oil, and condition determination is as follows:
Instrument is a Thermo TRACE GC Ultra-DSQ II makings logotype instrument.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, the results are shown in Table 1.
Table 1 Great Burdock Achene volatile oil component and relative content synopsis
By contrast, as can be seen, directly carrying out the volatile oil main component that supercritical extraction obtains is exactly oil substances.Volatile oil that the present invention's extraction obtains and wet distillation are relatively, have increase the fragrant and small molecular organic acid that reduces hormesis of cigarette ageing acid 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 by the lipid 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 and 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.As seen from the 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 is sent out more thoroughly, 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 30～90k/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 liquor, the precipitation thalline is even with physiological saline 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 geotrichum candidum fermentation Great Burdock Achene supercritical fluid extraction volatile oil 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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