CN102002437A - Method for extracting cigarette additives from pre-degreased burdock by ethanol and application thereof - Google Patents
Method for extracting cigarette additives from pre-degreased burdock by ethanol and application thereof Download PDFInfo
- Publication number
- CN102002437A CN102002437A CN 200910063801 CN200910063801A CN102002437A CN 102002437 A CN102002437 A CN 102002437A CN 200910063801 CN200910063801 CN 200910063801 CN 200910063801 A CN200910063801 A CN 200910063801A CN 102002437 A CN102002437 A CN 102002437A
- Authority
- CN
- China
- Prior art keywords
- extraction
- ethanol
- great burdock
- burdock achene
- cigarette
- 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.)
- Granted
Links
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 235000003130 Arctium lappa Nutrition 0.000 title claims abstract description 57
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 56
- 239000000654 additive Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- 240000005528 Arctium lappa Species 0.000 title claims description 55
- 235000008078 Arctium minus Nutrition 0.000 title abstract 4
- 239000000463 material Substances 0.000 claims abstract description 46
- 238000000605 extraction Methods 0.000 claims abstract description 42
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 17
- 238000009835 boiling Methods 0.000 claims abstract description 6
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 6
- 239000000284 extract Substances 0.000 claims description 36
- 230000000996 additive effect Effects 0.000 claims description 22
- 241000208125 Nicotiana Species 0.000 claims description 16
- 238000005238 degreasing Methods 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 13
- 230000006837 decompression Effects 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 235000012054 meals Nutrition 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 6
- 238000002791 soaking Methods 0.000 abstract description 5
- 235000013599 spices Nutrition 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 241000208843 Arctium Species 0.000 abstract 3
- 244000061176 Nicotiana tabacum Species 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 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 29
- 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 25
- 238000002481 ethanol extraction Methods 0.000 description 23
- 239000000203 mixture Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 8
- 239000000341 volatile oil Substances 0.000 description 8
- 238000005336 cracking Methods 0.000 description 7
- 239000000796 flavoring agent Substances 0.000 description 7
- 235000019634 flavors Nutrition 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
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- 239000003205 fragrance Substances 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 5
- -1 lignan compounds Chemical class 0.000 description 5
- OZJPLYNZGCXSJM-UHFFFAOYSA-N 5-valerolactone Chemical compound O=C1CCCCO1 OZJPLYNZGCXSJM-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- ZYEMGPIYFIJGTP-UHFFFAOYSA-N O-methyleugenol Chemical compound COC1=CC=C(CC=C)C=C1OC ZYEMGPIYFIJGTP-UHFFFAOYSA-N 0.000 description 4
- 229930013930 alkaloid Natural products 0.000 description 4
- 150000001720 carbohydrates Chemical class 0.000 description 4
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- 239000007789 gas Substances 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
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- 238000010561 standard procedure Methods 0.000 description 4
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- NZGWDASTMWDZIW-MRVPVSSYSA-N (+)-pulegone Chemical compound C[C@@H]1CCC(=C(C)C)C(=O)C1 NZGWDASTMWDZIW-MRVPVSSYSA-N 0.000 description 2
- VQKFNUFAXTZWDK-UHFFFAOYSA-N 2-Methylfuran Chemical compound CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 description 2
- KEFJLCGVTHRGAH-UHFFFAOYSA-N 2-acetyl-5-methylfuran Chemical compound CC(=O)C1=CC=C(C)O1 KEFJLCGVTHRGAH-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- ZFMSMUAANRJZFM-UHFFFAOYSA-N Estragole Chemical compound COC1=CC=C(CC=C)C=C1 ZFMSMUAANRJZFM-UHFFFAOYSA-N 0.000 description 2
- BJIOGJUNALELMI-ONEGZZNKSA-N Isoeugenol Natural products COC1=CC(\C=C\C)=CC=C1O BJIOGJUNALELMI-ONEGZZNKSA-N 0.000 description 2
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- 150000001299 aldehydes Chemical class 0.000 description 2
- USMNOWBWPHYOEA-UHFFFAOYSA-N alpha-thujone Natural products CC1C(=O)CC2(C(C)C)C1C2 USMNOWBWPHYOEA-UHFFFAOYSA-N 0.000 description 2
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- 239000002585 base Substances 0.000 description 2
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- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- BJIOGJUNALELMI-ARJAWSKDSA-N cis-isoeugenol Chemical compound COC1=CC(\C=C/C)=CC=C1O BJIOGJUNALELMI-ARJAWSKDSA-N 0.000 description 2
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- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 2
- 229940116837 methyleugenol Drugs 0.000 description 2
- PRHTXAOWJQTLBO-UHFFFAOYSA-N methyleugenol Natural products COC1=CC=C(C(C)=C)C=C1OC PRHTXAOWJQTLBO-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- BNWJOHGLIBDBOB-UHFFFAOYSA-N myristicin Chemical compound COC1=CC(CC=C)=CC2=C1OCO2 BNWJOHGLIBDBOB-UHFFFAOYSA-N 0.000 description 2
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
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- SATCULPHIDQDRE-UHFFFAOYSA-N piperonal Chemical compound O=CC1=CC=C2OCOC2=C1 SATCULPHIDQDRE-UHFFFAOYSA-N 0.000 description 2
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- 238000000197 pyrolysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- NNWHUJCUHAELCL-SNAWJCMRSA-N trans-isomethyleugenol Chemical compound COC1=CC=C(\C=C\C)C=C1OC NNWHUJCUHAELCL-SNAWJCMRSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
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- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical group CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 1
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 1
- IEMMBWWQXVXBEU-UHFFFAOYSA-N 2-acetylfuran Chemical compound CC(=O)C1=CC=CO1 IEMMBWWQXVXBEU-UHFFFAOYSA-N 0.000 description 1
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- CTHJQRHPNQEPAB-UHFFFAOYSA-N 2-methoxyethenylbenzene Chemical compound COC=CC1=CC=CC=C1 CTHJQRHPNQEPAB-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting cigarette additives from pre-degreased burdock by ethanol and application thereof, which belongs to the technical field of cigarette spice extraction. The method is carried out according to the following steps of: 1. crushing the burdock into coarse powder sieved by a sieve of 100 meshes, adding 6 to 10 times of quantity of medical level sherwood oil with the boiling range between 60 and 90 DEG C and soaking overnight, carrying out back flow extraction for 3 to 5h, filtering materials, remaining filter residue and drying the filter residue in the air; and 2. extracting the filter residue by 60 percent to 85 percent ethanol. The extraction method is the soaking extraction method or the ultrasonic extraction method or the back flow extraction method. A series of substances with better effect on the aesthetic quality of tobacco can be obtained through the extraction method, and the invention also enables medical ingredients of the burdock to be fully utilized.
Description
Technical field
The invention belongs to cigarette flavors extractive technique field, be a kind of specifically with after the pre-degreasing of plant amedica Great Burdock Achene, adopt soaking at room temperature or refluxing extraction or ultrasonic extraction, obtain the method for Great Burdock Achene ethanol extraction, and resulting ethanol extraction is 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, the applicant recognizes 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 a large amount of materials not to be employed in the Great Burdock Achene medicinal material, all be not used effectively as materials such as volatile oil, carbohydrate, amino acids, alkaloidss, have active effect and these materials are used for cigarette.But 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.
Have now and studies show that the essential substance basis of Great Burdock Achene medicinal material pharmacological action is Arctiin and aretigenin.The content of Arctiin is not less than 5.0% in " Pharmacopoeia of People's Republic of China (one one) " (version in 2005) regulation Great Burdock Achene.And relevant report is not seen in the application in cigarette of Arctiin and aretigenin.The structural formula of Arctiin and aretigenin is as follows:
Be Arctiin when wherein substituent R is for glucose, substituent R is an aretigenin during for hydrogen.Arctiin and aretigenin are the lignan compounds, are the dimers that the plain oxypolymerization of phenylpropyl alcohol forms.Can infer from its structure, can form phenylpropyl alcohol chlorins compound and derivative thereof after its burning cracking, and these compounds all be the cigarette perfume materials of using always.Therefore, the applicant infers Arctiin and the aretigenin utilize in the Great Burdock Achene, be used for cigarette flavors and make that to increase cigarette flavor after its cracking be 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.
Summary of the invention
Above-mentioned deficiency at prior art, one of the technical problem to be solved in the present invention provides a kind of method of extracting cigarette additive with ethanol after pre-degreasing the Great Burdock Achene, can from Great Burdock Achene, extract cigarette additive, wherein not only contain Arctiin and aretigenin, the material that also has volatile oil, carbohydrate, amino acids, alkaloids etc. not to be used effectively.Two of the technical problem to be solved in the present invention is that the above-mentioned cigarette additive that extracts from Great Burdock Achene should be improved quality of cigarette among cigarette.
Technical scheme of the present invention is: the method for extracting cigarette additive with ethanol after pre-degreasing the Great Burdock Achene is carried out according to the following steps successively:
[1], Great Burdock Achene was ground into the meal of 100 mesh sieves; The sherwood oil that adds 60-90 ℃ of medical grade boiling range that 6-10 doubly measures soaked 12-24 hour, and refluxing extraction 3-5h filters, and keeps filter residue and also dries;
[2], above-mentioned filter residue is extracted, extracting method is one of following method with the ethanol of 60%-85%:
(1) with the ethanol of above-mentioned filter residue and 60%-85% mixed according to mass ratio 1: 15-20, at room temperature soak and extract 2 times, each extraction time 36-48 hour, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is extraction using alcohol Great Burdock Achene cigarette additive;
(2) with the ethanol of above-mentioned filter residue and 60%-85% mixed according to mass ratio 1: 8-10, with ultrasonic extraction 2-3 time, ultrasonic power 150-300W, frequency 12-20KHz, each extraction time 0.5-1 hour, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is extraction using alcohol Great Burdock Achene cigarette additive;
(3) with the ethanol of above-mentioned filter residue and 60%-85% mixed, refluxing extraction 2-3 time, 85 ℃ of reflux temperatures according to mass ratio 1: 5-10, each extraction time 1-3 hour, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is extraction using alcohol Great Burdock Achene cigarette additive.
Extract the application of cigarette additive after pre-degreasing the Great Burdock Achene with ethanol: with the prepared extraction using alcohol Great Burdock Achene of aforesaid method cigarette additive, the alcohol dilution with 95% becomes 10%, and the 0.02-0.1% according to pipe tobacco weight adds in the pipe tobacco then.
Except as otherwise noted, percentage ratio of the present invention and ratio all refer to weight percentage and weight ratio.
Advantage of the present invention:
The present invention adopts sherwood oil degreasing in advance can effectively remove the lipid composition, promotes the quality of Great Burdock Achene ethanol extraction as cigaret additive.Carrying out the effect of Great Burdock Achene ethanol extraction in cigarette that extraction using alcohol obtains after the degreasing again is better than not degreasing greatly and directly carries out the Great Burdock Achene ethanol extraction that extraction using alcohol obtains.
Adopt the medical grade sherwood oil can guarantee that the ethanol extraction that obtains meets the cigarette quality standard.
In the Great Burdock Achene ethanol extraction main component Arctiin that employing the inventive method obtains and the split product of aretigenin the flavour ingredient that often uses in a lot of tobacco blending is arranged, the fragrant coordination of cigarette enriched when tobacco was burnt and sucked, and fragrance matter promotes.Opened up the new purposes of Arctiin and aretigenin.
The Great Burdock Achene ethanol extraction that adopts the inventive method to obtain also contains materials such as volatile oil, Arctiin and aretigenin, carbohydrate, amino acids, alkaloids, all be the material that the aesthetic quality of tobacco is had better effect, the present invention is fully used the composition of Great Burdock Achene medicinal material.
Embodiment
Below in conjunction with embodiments of the invention the relevant technologies problem is described in further detail.
Embodiment 1 was ground into the Chinese medicinal materials Great Burdock Achene meal of 100 mesh sieves; Boiling range 60-90 ℃ the medical grade sherwood oil soaked overnight that adds 6 times of amounts, refluxing extraction 5h degreasing is filtered, and the reservation filter residue also dries; The ethanol of filter residue and 85% is carried out soaking at room temperature extraction 2 times according to 1: 20 ratio of mass ratio, each time of soaking extraction is 48 hours, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is Great Burdock Achene ethanol extraction cigarette additive.
The Great Burdock Achene ethanol extraction is become 10% solution with 95% alcohol dilution, add in the high-grade cigarette pipe tobacco according to 0.02% of pipe tobacco weight then, smoke panel test according to national standard method after making cigarette.Smoking result is: the effect of tangible flavouring and lifting fragrance matter is arranged.
Embodiment 2 was ground into the meal of 100 mesh sieves with the Chinese medicinal materials Great Burdock Achene, added boiling range 60-90 ℃ medical grade sherwood oil soaked overnight of 8 times of amounts, and refluxing extraction 4h degreasing is filtered, and kept filter residue and also dried; The ethanol of filter residue and 60% is carried out ultrasonic extraction 3 times according to 1: 10 ratio of mass ratio, and the time of each ultrasonic extraction is 0.5 hour, ultrasonic power 200W, frequency 15KHz.Filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is Great Burdock Achene ethanol extraction cigarette additive.
The Great Burdock Achene ethanol extraction is become 10% solution with 95% alcohol dilution, add in the middle-grade cigarette shreds according to 0.04% of pipe tobacco weight then, smoke panel test according to national standard method after making cigarette.Smoking result is: increase the rich of flue gas concentration and fragrance, promote fragrance matter.
Embodiment 3 was ground into the meal of 100 mesh sieves with the Chinese medicinal materials Great Burdock Achene, added boiling range 60-90 ℃ medical grade sherwood oil soaked overnight of 10 times of amounts, and refluxing extraction 3h degreasing is filtered, and kept filter residue and also dried; The ethanol of filter residue and 70% is carried out refluxing extraction 3 times according to 1: 5 ratio of mass ratio, 85 ℃ of reflux temperatures, the time of each refluxing extraction is 2 hours.Filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is Great Burdock Achene ethanol extraction cigarette additive.
The present invention becomes 10% solution with the Great Burdock Achene ethanol extraction with 95% alcohol dilution, adds in the Low-end Cigarettes pipe tobacco according to 0.1% of pipe tobacco weight then, smokes panel test according to national standard method after making cigarette.Smoking result is: increase flue gas concentration, promote perfume quantity.
The applicant before making the present invention through the further investigation, recognize that unemployed composition in the Great Burdock Achene medicinal material all has better action to the aesthetic quality of tobacco: glucide: can produce acidic substance on the one hand, the alkalescence that suppresses flue gas neutral and alkali material, make the acid base equilibrium appropriateness of flue gas, reduce pungency, produce gratifying jealous; On the other hand, prop up in the process of burning and sucking in heating and cigarette, sugar is the important as precursors that forms aroma substance, when temperature at 300 degree when above, pyrolysis forms multiple aroma substance separately, and wherein most important have a furan derivatives, carbonyl compound such as simple ketone and aldehydes.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, and these materials have strong fragrance, is the material of the frequent increase cigarette perfume (or spice) that uses in the cigarette blending.The amino acids material: the burning of an amount of amino acid produces nitrogenous compound, and flue gas is enriched, energetically; Simultaneously can also and reducing sugar between the Maillard reaction takes place, generate have sweet, roasting, puffed rice, nut, the compound of feature fragrance such as cheese.Alkaloids substance: be similar to the effect of nicotine, can effectively remedy or improve the strength of cigarette.
Therefore, consider that the materials such as volatile oil, Arctiin and aretigenin that are primarily aimed in the Great Burdock Achene extract, be used for cigarette flavors, can increase cigarette flavor.And materials such as volatile oil, Arctiin and aretigenin have solvability preferably in ethanol, also can obtain materials such as Arctiin and aretigenin simultaneously in extract.Therefore, consider to extract as solvent with ethanol.In the process of materials such as extraction using alcohol volatile oil, Arctiin and aretigenin, the material that carbohydrate, amino acids, alkaloids etc. have a better effect to the aesthetic quality of tobacco has part and is extracted simultaneously, thereby the composition of Great Burdock Achene medicinal material is fully used.Also have inexpensive advantage with extraction using alcohol, therefore help the popularization of industrial application.
But, also containing the lipid composition of the 26-30% that has an appointment in the Great Burdock Achene, content is very high, comprises palmitic acid, stearic acid, oleic acid, linolic acid, linolenic acid etc.And these lipid compositions add in the cigarette, can bring more serious assorted gas, stimulation and oral cavity residual, influence the cigarette quality.If directly extract with ethanol, these lipid compositions have part and are extracted simultaneously, thereby have influenced the effect of extract in cigarette.Therefore before extraction using alcohol, adopt sherwood oil to carry out degreasing, thereby obtain being applicable to the additive of cigarette.
The contriver has carried out the volatile component evaluation with the gas chromatography instrument to the Great Burdock Achene ethanol extraction, 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 applicant adopts the method for distillation extraction simultaneously to extract and the ethanol extraction of the present invention that direct extraction using alcohol obtains, and has carried out volatile component GC/MS and has analyzed contrast, and the area normalization quantitative result sees Table 1.
Table 1 Great Burdock Achene ethanol extraction volatile component and relative content synopsis
By contrast, the ethanol extraction that the present invention obtains compares with the extract that direct extraction using alcohol obtains, and the principal constituent pulegone has inhibition in tobacco stimulate, and covers assorted gas, improves the effect of mouthfeel, and content is higher among the present invention; And palmitic acid, stearic acid etc. can bring more serious assorted gas, stimulation and oral cavity residual, influence cigarette quality fatty acid component content and obviously reduce.Therefore, effect therefore can be better in cigarette flavoring for the ethanol extraction that obtains of the present invention extraction.
Arctiin and aretigenin Determination on content in the Great Burdock Achene ethanol extraction that the contriver obtains the present invention with high performance liquid chromatography, condition determination is as follows:
Instrument is Dionex 3000 highly effective liquid phase chromatographic systems.Chromatographic condition: Diamonsil TM (diamond) chromatographic column (4.6mm * 250mm, 5 μ m); Detect wavelength 280nm; 30 ℃ of column temperatures; Flow velocity 1.0ml/min; Sample size: 10 μ l.Condition of gradient elution is: acetonitrile-water, elution program (seeing Table 2).
Table 2 gradient elution program
| Time (min) | Acetonitrile (%) | Water (%) |
| ?0-8 | 30-25 | 70-75 |
| ?8-13 | 25-24 | 75-76 |
| ?13-40 | 24-70 | 76-30 |
Arctiin and aretigenin assay result such as following table 3 in the Great Burdock Achene ethanol extraction of the present invention.
Table 3 Arctiin and aretigenin assay result
| Arctiin (%) | Aretigenin (%) | |
| Embodiment 1 | 5.86 | 1.17 |
| Embodiment 2 | 6.12 | 1.05 |
| Embodiment 3 | 6.24 | 1.13 |
The contriver studies the thermal cracking products of Arctiin, and condition determination is as follows:
Instrument: Pyroprobe 2000 thermo-cracking instrument (U.S. CDS company), DSQ II gas chromatograph-mass spectrometer (U.S. Thermo Fisher company).Thermo-cracking atmosphere: nitrogen.Thermo-cracking probe (pyrolysis head) initial temperature: 30 ℃, rise to 300 ℃ of outlet temperatures, 600 ℃ and 900 ℃, time length 10s respectively with 20 ℃/ms speed.DB-5ms 30 * 0.25mm * 0.25 μ m; Temperature programming: 40 ℃ (keeping 1min), be warming up to 100 ℃ (keeping 1min) with 2 ℃/min, with 8 ℃/min, be warming up to 280 ℃ (keeping 5min); Injector temperature: 260 ℃; Interface temperature: 280 ℃; Input mode: shunting, flow velocity 1.0ml/min; Ionization energy: 70eV.Sweep limit: 35-400amu, standard mass spectral database: NIST98 and WILEY275 spectrum storehouse.Area normalization is quantitative.
Arctiin is thermo-cracking result under the differing temps such as following table 4 in nitrogen environment.
The thermo-cracking primary product result (%) of table 4 Arctiin
| Sequence number | Composition | 300℃ | 600℃ | 900℃ |
| 1 | The 2-methyl furan | Do not detect | 0.55 | 0.38 |
| 2 | 2-vinyl furans | Do not detect | 0.17 | Do not detect |
| 3 | Toluene | Do not detect | 1.21 | 1.56 |
| 4 | Furfural | 12.78 | 8.92 | 4.59 |
| 5 | 2-propenyl furans | Do not detect | 0.11 | 0.64 |
| 6 | 2-propyl group furans | Do not detect | 1.35 | 1.42 |
| 7 | The a-angelica lactone | Do not detect | 2.24 | 0.91 |
| 8 | 2-cyclopentenes-1, the 4-diketone | Do not detect | 0.56 | 0.23 |
| 9 | The 2-acetyl furan | Do not detect | 0.59 | 0.28 |
| 10 | Phenyl aldehyde | Do not detect | 3.03 | 1.25 |
| 11 | 5 methyl furfural | Do not detect | 1.56 | 0.44 |
| 12 | Cumarone | Do not detect | 0.37 | 0.11 |
| 13 | 5-methyl-2-acetyl furan | Do not detect | 0.21 | Do not detect |
| 14 | Phenol | Do not detect | 0.26 | 0.31 |
| 15 | Pu'er ketone | Do not detect | 3.56 | 2.61 |
| 16 | Valerolactone | 15.61 | 6.52 | 5.69 |
| 17 | Adjacent Vinyl toluene | Do not detect | 0.24 | 6.42 |
| 18 | 1-proyl toluene | Do not detect | Do not detect | 4.53 |
| 19 | Methyl phenyl ketone | Do not detect | 2.24 | 2.65 |
| 20 | Methyl benzoate | Do not detect | 0.68 | 0.31 |
| 21 | Estragole | Do not detect | 6.61 | 5.47 |
| 22 | Paracymene | Do not detect | 2.65 | 4.41 |
| 23 | Methyleugenol | 20.56 | 4.75 | 5.41 |
| 24 | Oxymethoxyallylbenzene | 16.52 | 6.42 | 0.23 |
| 25 | To methoxy styrene | Do not detect | 0.11 | 7.83 |
| 26 | 2,6,6-trimethylammonium-6-vinyl-dihydropyrane-3-ketone | Do not detect | 0.89 | Do not detect |
| 27 | Isoeugenol | 15.79 | 8.37 | 9.77 |
| 28 | Phenylformic acid | Do not detect | 4.78 | 6.32 |
| 29 | 1, the 2-benzisothiazole | Do not detect | Do not detect | 0.23 |
| 30 | Benzothiazole | Do not detect | 0.24 | Do not detect |
| 31 | Linalool monoxide | Do not detect | 1.83 | 2.35 |
| 32 | The methyl isoeugenol | Do not detect | 6.11 | 1.88 |
| 33 | Benzylideneacetone | Do not detect | 0.47 | 0.69 |
| 34 | Piperonylaldehyde | 15.62 | 12.36 | 9.38 |
| 35 | Trans linalool oxide | Do not detect | 2.18 | 1.17 |
| 36 | Myristicin | Do not detect | 6.49 | 4.22 |
| 37 | Diphenylene-oxide | Do not detect | Do not detect | 1.34 |
| 38 | Tolane | Do not detect | Do not detect | 0.95 |
| 39 | 1, the 2-tolane | Do not detect | Do not detect | 0.31 |
As seen, the Arctiin composition that content is bigger in the thermal cracking products under the differing temps mainly contains: furfural, valerolactone, methyleugenol, oxymethoxyallylbenzene, isoeugenol, piperonylaldehyde etc. from last table.These compositions all have the effect that increases cigarette perfume (or spice) preferably.The structure and the Arctiin of aretigenin are similar, have just lacked a glucosyl group in the structure, and therefore, its split product and Arctiin are similar, do not give unnecessary details.
The contrast of smokeing panel test of extract that the applicant obtains direct extraction using alcohol and ethanol extraction of the present invention is smoked panel test and is carried out according to national standard method, and 7 people form the group of smokeing panel test, 2 national judging panels, 5 provincial judging panels, smoking result such as following table 5.As seen from the table, ethanol extraction of the present invention, apply with pipe tobacco after, the aesthetic quality that can improve cigarette.
Table 5 contrast table of smokeing panel test
Claims (2)
1. one kind is extracted the method for cigarette additive with ethanol the Great Burdock Achene after pre-degreasing, it is characterized in that described method carries out according to the following steps successively:
[1], Great Burdock Achene was ground into the meal of 100 mesh sieves; The sherwood oil that adds 60-90 ℃ of medical grade boiling range that 6-10 doubly measures soaked 12-24 hour, and refluxing extraction 3-5h filters, and keeps filter residue and also dries;
[2], above-mentioned filter residue is extracted, extracting method is one of following method with the ethanol of 60%-85%:
(1) with the ethanol of above-mentioned filter residue and 60%-85% mixed according to mass ratio 1: 15-20, at room temperature soak and extract 2 times, each extraction time 36-48 hour, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is extraction using alcohol Great Burdock Achene cigarette additive;
(2) with the ethanol of above-mentioned filter residue and 60%-85% mixed according to mass ratio 1: 8-10, with ultrasonic extraction 2-3 time, ultrasonic power 150-300W, frequency 12-20KHz, each extraction time 0.5-1 hour, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is extraction using alcohol Great Burdock Achene cigarette additive;
(3) with the ethanol of above-mentioned filter residue and 60%-85% mixed, refluxing extraction 2-3 time, 85 ℃ of reflux temperatures according to mass ratio 1: 5-10, each extraction time 1-3 hour, filter, filtrate decompression is condensed into medicinal extract shape material, and gained medicinal extract shape material is extraction using alcohol Great Burdock Achene cigarette additive.
2. application of after pre-degreasing, extracting cigarette additive with ethanol the Great Burdock Achene, it is characterized in that: with the prepared extraction using alcohol Great Burdock Achene of the method for claim 1 cigarette additive, alcohol dilution with 95% becomes 10%, and the 0.02-0.1% according to pipe tobacco weight adds in the pipe tobacco then.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103844346A (en) * | 2014-03-04 | 2014-06-11 | 江苏中烟工业有限责任公司 | Burdock root ethanol extract and application thereof in tobacco |
| CN103859578A (en) * | 2014-03-04 | 2014-06-18 | 江苏中烟工业有限责任公司 | Extracting method of burdock crude polysaccharide and application of burdock crude polysaccharide to tobacco |
| CN104560399A (en) * | 2014-12-16 | 2015-04-29 | 湖北中烟工业有限责任公司 | Method for purifying jasmine flower extract for cigarettes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569138A (en) * | 2004-05-13 | 2005-01-26 | 上海交通大学 | Preparation method of arctium fruit extract for decreasing blood sugar |
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2009
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103844346A (en) * | 2014-03-04 | 2014-06-11 | 江苏中烟工业有限责任公司 | Burdock root ethanol extract and application thereof in tobacco |
| CN103859578A (en) * | 2014-03-04 | 2014-06-18 | 江苏中烟工业有限责任公司 | Extracting method of burdock crude polysaccharide and application of burdock crude polysaccharide to tobacco |
| CN103859578B (en) * | 2014-03-04 | 2016-05-18 | 江苏中烟工业有限责任公司 | The extracting method of the thick polysaccharide of a kind of burdock and the application in tobacco thereof |
| CN104560399A (en) * | 2014-12-16 | 2015-04-29 | 湖北中烟工业有限责任公司 | Method for purifying jasmine flower extract for cigarettes |
| CN104560399B (en) * | 2014-12-16 | 2017-11-07 | 湖北中烟工业有限责任公司 | A kind of purification process of cigarette jasmine flower extract |
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