CN1488300A - Cigarette additive extracted from natural plant, and extracting method and use in cigarette thereof - Google Patents
Cigarette additive extracted from natural plant, and extracting method and use in cigarette thereof Download PDFInfo
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- CN1488300A CN1488300A CNA031402291A CN03140229A CN1488300A CN 1488300 A CN1488300 A CN 1488300A CN A031402291 A CNA031402291 A CN A031402291A CN 03140229 A CN03140229 A CN 03140229A CN 1488300 A CN1488300 A CN 1488300A
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Abstract
The invention is a cigarette addition extracted form natural plant, extracting method and application in cigarette. The cigarette contains 5%-100% total coumarin ramification extract, 0-95% grass coral extract, and 0-95% dandelion extract. The total coumarin ramification can be obtained by the method of first extracting or digesting by water and organic solvent, or extracting by diacolation, or by the method of extracting to separate by supercritical CO2 to refine or recrystallize, or by the method of directly extracting by supercritical CO2. It can obviously reduce harm of cigarette and enhance safety of cigarette when added in cigarette.
Description
Technical field
The present invention relates to a kind of cigarette additives and extracting method thereof and the application in cigarette thereof.
Background technology
The harmfulness of smoking health, in the smog of cigarette, contain multiple noxious material, can cause cancer, arterial thrombotic disease, immunologic function reduces, breathing problem, increasing of disease incidences such as hypogona dism, but for long-term smoker, smoking cessation is often very difficult, external researcher generally is devoted to improve the prescription of tobacco, reduce the wherein content of tar, the researcher of China then utilizes the treasure-house of traditional traditional Chinese medicine and pharmacy, the plant or its extract or its volatile oil that add Chinese herbal medicine in the pipe tobacco, so that the smoker can suck the effective medicinal components in the Chinese herbal medicine in smoking process, thus the harm of weakening or minimizing cigarette.This is the very important approach that tobacco business reduces cigarette harm, also is that development has the new measure of China's characteristic cigarette.
Summary of the invention
First purpose of the present invention is to provide a kind of cigarette additives from extracted form natural plant, and this additive can reduce the harm of cigarette to human body, thereby improves the security of cigarette.
Second purpose of the present invention is to provide the extracting method of above-mentioned cigarette additives.
The 3rd purpose of the present invention is above-mentioned cigarette additives from extracted form natural plant is applied to cigarette.
First purpose of the present invention is achieved in that cigarette additives of the present invention contains the general coumarin derivative extract of 5%-100%, the Herba Pileae Scriptae extract of 0-95%, the dandelion extract of 0-95%;
The extract of described general coumarin derivative is from the Carrot family plant, legume, extract in the plant of one or more of rutaceae, the plant part of being got is complete stool or its root of plant, stem, branch, leaf, flower, fruit, seed, the Carrot family plant is as glehnia littoralis Glehnia Littoralis Fr.Schmidt ex Miq, Imperatoria ostruthium Peucedanumosthru thium (L.) Koch, RADIX PEUCEDANI Peucedanum Praeruptorum Dunn, RADIX PEUCEDANI Peucedanum decursivum Maxim, Angelica pubescens Angelica pubescensMaxim, root of Dahurain angelica Angelica dahurica (Fisch.ex Hoffm..) Benth.et Hook.f., Radix angelicae dahuricae Angelica dahurica (Fisch..ex Hoffm.) Benth.et Hook.f.Varformosana (Boiss.) shan et Yuan, cnidium monnieri Cnidium monnieri (L.) Cuss., legume such as Psoralea corylifolia Psoralea Corylifolia L., rutaceae such as anistree Calusena lansium Clausena anisata Oliv., single leaf rue Haplophyllum bungei Trautv; The main component of general coumarin derivative extract is the derivative of general coumarin, and the derivative of general coumarin is one or more the compound in following formula (1), the formula (2):
Formula (1)
R
1＝H，OH，OCH
3；
Described Herba Pileae Scriptae extract is to extract from the herb of golden grain Zhu Ke plant plait coral Sarcandra glabra (Thunb.) Nakai drying and get, and its main component is general coumarin lactone, lactone, flavones and organic acid, as isofraxidin isofraxidin
Fumaric acid (Fumaric acid)
Described dandelion extract is that the dry herb by feverfew dandelion Taraxacum mongolicumHand.-Mazz. and congener thereof extracts and gets.
Second purpose of the present invention is achieved in that
The extracting method of general coumarin derivative extract has three kinds, and first kind of extracting method comprises the steps:
(1) gets one or more plant complete stool drying in Carrot family plant, legume, rutaceae and the equal platymiscium, pulverize, water or pure heating and refluxing extraction, or lixiviate, or, extract twice, each 1～24 hour with the percolation extraction, used alcohol is ethanol or methyl alcohol, or they and the formulated concentration of water are 50～100% alcoholic solution;
(2) extract is filtered, be condensed into paste after reclaiming solvent, this medicinal extract extracts with organic solvent again, the same or extraction of extracting method, used organic solvent is selected oxolane for use, hexane, benzinum, benzene, chloroform, ether, acetone, ethyl acetate, ethanol, methyl alcohol, extract reclaims solvent, as do not have crystallization and separate out, extract is handled with ammoniacal liquor or dilute alkaline soln again, washes with water to neutrality, reclaim solvent again, place about 0 ℃, separate out if any crystal, then the leaching crystal, use one or more recrystallizations of above-mentioned organic solvent again, promptly get general coumarin derivative extract; As do not have crystal and separate out, then carrying out chromatography, adsorbent is silica gel or aluminium oxide, eluant, eluent is the mixed solution of one or more different proportions of above-mentioned organic solvent, and eluent reclaims solvent, is placed with crystal about 0 ℃ and separates out, with above-mentioned method recrystallization, promptly.
The extracting method of second kind of general coumarin derivative extract comprises the steps:
(1) gets one or more plant complete stool drying in Carrot family plant, legume, rutaceae and the equal platymiscium, pulverize, water or pure heating and refluxing extraction, or lixiviate, or, extract twice, each 1～24 hour with the percolation extraction, used alcohol is ethanol or methyl alcohol, or they and the formulated concentration of water are 50～100% alcoholic solution;
(2) extract is filtered, be condensed into paste behind the recovery solvent, separate with supercritical carbon dioxide extracting again, obtain crystal and re-refine or be recrystallized, promptly.
The extracting method of the third general coumarin derivative extract comprise the steps: to get in Carrot family plant, legume, rutaceae and the equal platymiscium one or more plant drying, be ground into meal, extract with supercritical carbon dioxide, obtain crystal and re-refine or be recrystallized, promptly.
Herba Pileae Scriptae extract and dandelion extract can adopt following three kinds of methods to extract:
(1) Chloranthus glaber or dandelion plant herb drying, pulverizing, water or pure heating and refluxing extraction, or lixiviate, or percolation extracts, and extracts secondary, each 1～24 hour, used alcohol was the alcoholic solution of ethanol or methyl alcohol or 50～100% concentration that are made into water; Extract is filtered, and decompression or normal pressure reclaim solvent, and extract is condensed into paste, this paste water, alcohol or acetone, ethyl acetate repeated treatments, reclaim solvent, are concentrated into paste promptly.
(2) Chloranthus glaber or dandelion plant herb drying, be ground into meal, extract with supercritical carbon dioxide.
(3) in the aforementioned first method through the paste of water or alcohol extracting gained, promptly with supercritical carbon dioxide treatment.
Cigarette additives of the present invention is applied in the cigarette, be to be cigarette additives and concentration that the ethanolic solution of 50%-95% is mixed with cigarette additive and is added into and makes health cigarette in the cigarette, the adding proportion of this additive is that the 0.01%-10% of pipe tobacco weight is better.
Contain multiple beneficial such as general coumarin derivative, isofraxidin, fumaric acid in the active material of health in general coumarin derivative extract, Herba Pileae Scriptae extract, the dandelion extract, have physiology and pharmacological effect widely, can fully coordinate with pipe tobacco aspect color, smell and taste, wherein the easy gasification of active ingredient enters respiratory tract with main flume.Utilize the HPLC method that the general coumarin derivative in the cigarette additives of the present invention has been carried out assay determination, the result shows: the general coumarin derivative content is the cigarette that 18.55 μ g/ prop up, the content of general coumarin derivative is that 5.22 μ g/ prop up in its flue gas, and the rate of transform is more than 28.14%.Further experiment shows: the existence of general coumarin derivative is also arranged in the serum of chronic suction experiment cigarette mouse, illustrate that the main component general coumarin derivative of cigarette additives of the present invention can be absorbed in the blood by oral cavity etc.
The applicant has carried out comprehensive test from aspects such as active ingredient transfer, flue gas analysis, security biological assessment and effect detections to cigarette additives of the present invention, provides direct, objective and ample evidence cigarette additives of the present invention is applied to can reduce cigarette harm in the cigarette.
Result of study shows: cigarette additives of the present invention has an obvious blocking effect to volatile nitrosamine and the distinctive nitrosamine of tobacco are synthetic; Mutagenicity to benzo [a] pyrene has significant inhibitory effect.Cigarette additive is being higher than when using 1000 times of concentration, and toxic and side effect is not all observed in animal and cell in vitro test, shows cigarette additives safety non-toxic of the present invention.
On this basis, the applicant studies the effect that cigarette additives of the present invention is applied to can to reduce in the cigarette cigarette harm, the cigarette that has added additive of the present invention has been carried out the smoke chemistry analysis and the biological assessment of system.The result shows: compare with the contrast cigarette that does not add additive of the present invention, can significantly alleviate bad reactions such as caused by smoking cough, asthma, stasis of blood phlegm, obviously reduce the incidence of disease of breathing problem; The free radical level reduces more than 20%; Make the time and the deadly smoking capacity of mouse and rat smoking acute death increase about 60% and 30% respectively; Particularly when smoking control group cigarette treated animal was all dead, additive cigarette treated animal survival rate was up to more than 85%; The acute toxic reaction of mouse obviously alleviates, and the prolonged survival period that shows animal is more than 1 times, and deadly smoking capacity significantly increases; Lung tissue pathology observed result shows: be all the acute or chronic lethal animal of smoking, experiment cigarette group lung tissue degree of injury obviously alleviates, and shows that lymphocytic infiltration, alveolus wall thicken, hemorrhage, tracheaectasy, epithelium attenuation, lung sac bubble and manage multinomial pathology damage index such as all oedema all significantly better than contrast cigarette group; Significantly sister chromosome exchanges and the marrow microkernel incidence due to the inhibition cigarette condensation product; Make that the dosage of SHE and the death of BEAS-2B cell half is increased to 1.7 and 4 times respectively due to the cigarette smoke, the level of bringing out the ROS that cell produces obviously reduces, and shows H in cell
2O
2And O
2 -Level reduces for work; With with quality contrast cigarette relatively, cytotoxicity has reduced 2-4 doubly, the cellular oxidation that cigarette smoke brings out, cell membrane damage, chromogene sudden change and cell transformation effect obviously reduce.
Above result of study shows: the cigarette additives of using the present inventor can significantly reduce the harm of cigarette, the security that obviously improves cigarette.
The invention will be further described below in conjunction with embodiment.
The specific embodiment
Embodiment one:
The preparation of general coumarin derivative extract:
Get the Psoralea corylifolia seed, drying is ground into meal, mix wetly with 60% ethanol, well-established law is packed in the diacolation cylinder, and lixiviate is diacolation after 12 hours, collect the percolate of 10 times of amounts, decompression recycling ethanol leaves standstill, the collecting precipitation thing, sediment is handled with methyl alcohol, left standstill, promptly have crystal to separate out, collect, being recrystallized routinely with methyl alcohol promptly gets general coumarin derivative extract.
Getting above gained general coumarin derivative extract 1400 μ g, to dissolve in 1ml concentration as cigarette additives be 90% ethanolic solution, is mixed with the cigarette additive that cigarette additives concentration is 1400 μ g/ml.Cigarette additive is added in the pipe tobacco with table perfume (or spice), and the addition of cigarette additives is 0.2% of a pipe tobacco weight, and cigarette process is made a health care cigarette routinely, the heavy 0.7g of Linear Leaf Speedwell cigarette, and every health care cigarette contains additive 1400 μ g.
Embodiment two:
The preparation of general coumarin derivative extract:
(1) get the seed of Carrot family plant cnidium monnieri, drying is pulverized, and extracts secondary with 95% alcohol reflux earlier, and each 2 hours, extract merged and filters, and is condensed into paste behind the recovery solvent;
(2) paste is separated with supercritical carbon dioxide extracting, obtain crystal and re-refine, promptly get general coumarin derivative extract.
The general coumarin derivative extract 70 μ g that get gained make cigarette additive by the method for embodiment one and are added in the pipe tobacco, make a health care cigarette, the heavy 0.7g of Linear Leaf Speedwell cigarette, adopting embodiment one cigarette additive 90% ethanolic solution to change concentration into is 70% ethanolic solution, and the adding proportion of cigarette additives is 0.01% of a pipe tobacco weight.
Embodiment three:
The preparation of general coumarin derivative extract: get the root of the Carrot family plant root of Dahurain angelica, drying is ground into meal, extracts with supercritical carbon dioxide, leaves standstill, and gets its precipitate and gets general coumarin derivative extract, re-refines promptly.
The preparation of Herba Pileae Scriptae extract and dandelion extract: Chloranthus glaber or dandelion plant herb drying, pulverizing, elder generation's water heating and refluxing extraction 2 times, each 2 hours, merging extract filters, decompression is condensed into rare paste, this paste Ethanol Treatment, handles with ethyl acetate again, reclaim solvent, be concentrated into paste and promptly get Herba Pileae Scriptae extract or dandelion extract.
Get above gained general coumarin derivative extract 800 μ g, Herba Pileae Scriptae extract 2000 μ g, dandelion extract 5200 μ g, method by embodiment one is added in the pipe tobacco, make a health care cigarette, the weight percentage of cigarette additives is 1.14% in this health care cigarette.
Embodiment four:
The preparation of Herba Pileae Scriptae extract: get Chloranthus glaber plant herb, dry, be ground into meal, extract with supercritical carbon dioxide, promptly get Herba Pileae Scriptae extract.
The preparation of general coumarin derivative extract is with embodiment one.
Get above-mentioned gained Herba Pileae Scriptae extract 66.5mg and general coumarin derivative extract 3.5mg, method by embodiment one is made cigarette additives, be added into then in the pipe tobacco, make a health care cigarette, the weight percentage of cigarette additives is 10% in this health care cigarette.
Embodiment five:
The preparation of dandelion extract: preceding step is with embodiment three, and the paste of water, alcohol extract gained promptly gets dandelion extract with supercritical carbon dioxide treatment.
Get above-mentioned gained dandelion extract 6.65mg and general coumarin derivative extract 0.35mg, method by embodiment one is made cigarette additives, be added into then in the pipe tobacco, make a health care cigarette, the weight percentage of cigarette additives is 1% in this health care cigarette.
Dandelion extract also can adopt the extracting method of Herba Pileae Scriptae extract among the embodiment four and gets in the present embodiment, and Herba Pileae Scriptae extract can adopt the extracting method of dandelion extract in the present embodiment and gets among the embodiment four.
Claims (7)
1. the cigarette additives from extracted form natural plant is characterized in that: contain the general coumarin derivative extract of 5%-100%, the Herba Pileae Scriptae extract of 0-95%, the dandelion extract of 0-95%;
The extract of described general coumarin derivative is to extract from one or more plant of Carrot family plant, legume, rutaceae, the plant part of being got is the complete stool of plant or its root, stem, branch, leaf, flower, fruit, seed, its main component is the general coumarin derivative, and the general coumarin derivative is one or more the compound in formula (1), the formula (2):
Formula (1)
R
1＝H，OH，OCH
3；
Formula (2)
Described Herba Pileae Scriptae extract is to extract from the herb of Chloranthus glaber drying and get, and its main component is general coumarin lactone, flavones and organic acid, comprises isofraxidin, fumaric acid;
Described dandelion extract is that the dry herb by dandelion and congener thereof extracts and gets.
2. the cigarette additives from extracted form natural plant according to claim 1, it is characterized in that: described Carrot family plant comprises glehnia littoralis, Imperatoria ostruthium, RADIX PEUCEDANI, RADIX PEUCEDANI, Angelica pubescens, the root of Dahurain angelica, Radix angelicae dahuricae, cnidium monnieri, described legume comprises Psoralea corylifolia, described rutaceae comprises anistree Calusena lansium, single leaf rue, and congener.
3. the extracting method of the described cigarette additives of claim 1 is characterized in that the extraction step of described general coumarin derivative extract is as follows:
(1) gets one or more plant drying in Carrot family plant, legume, rutaceae and the equal platymiscium, pulverize, water or pure heating and refluxing extraction, or lixiviate, or, extract twice, each 1～24 hour with the percolation extraction, used alcohol is ethanol or methyl alcohol, or they and the formulated concentration of water are 50～100% alcoholic solution;
(2) extract is filtered, be condensed into paste after reclaiming solvent, this medicinal extract extracts with organic solvent again, the same or extraction of extracting method, used organic solvent is selected oxolane for use, hexane, benzinum, benzene, chloroform, ether, acetone, ethyl acetate, ethanol, methyl alcohol, extract reclaims solvent, as do not have crystallization and separate out, extract is handled with ammoniacal liquor or dilute alkaline soln again, washes with water to neutrality, reclaim solvent again, place about 0 ℃, separate out if any crystal, then the leaching crystal, use one or more recrystallizations of above-mentioned organic solvent again, promptly get general coumarin derivative extract; As do not have crystal and separate out, then carrying out chromatography, adsorbent is silica gel or aluminium oxide, eluant, eluent is the mixed solution of one or more different proportions of above-mentioned organic solvent, and eluent reclaims solvent, is placed with crystal about 0 ℃ and separates out, with above-mentioned method recrystallization, promptly.
4. the extracting method of the described cigarette additives of claim 1 is characterized in that the extraction step of described general coumarin derivative extract is as follows:
(1) gets one or more plant drying in Carrot family plant, legume, rutaceae and the equal platymiscium, pulverize, water or pure heating and refluxing extraction, or lixiviate, or, extract twice, each 1～24 hour with the percolation extraction, used alcohol is ethanol or methyl alcohol, or they and the formulated concentration of water are 50～100% alcoholic solution;
(2) extract is filtered, be condensed into paste behind the recovery solvent, separate with supercritical carbon dioxide extracting again, obtain crystal and re-refine or be recrystallized, promptly.
5. the extracting method of the described cigarette additives of claim 1, the extraction step that it is characterized in that described general coumarin derivative extract is as follows: get in Carrot family plant, legume, rutaceae and the equal platymiscium one or more plant drying, be ground into meal, extract with supercritical carbon dioxide, obtain crystal and re-refine or be recrystallized, promptly.
6. the application of the described cigarette additives of claim 1 in cigarette.
7. the application of cigarette additives according to claim 6 in cigarette is characterized in that: the 0.01%-10% ratio of this additive in pipe tobacco weight is added in the pipe tobacco.
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| CN 03140229 CN1225998C (en) | 2003-08-19 | 2003-08-19 | Cigarette additive extracted from natural plant, and extracting method and use in cigarette thereof |
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| CN 03140229 CN1225998C (en) | 2003-08-19 | 2003-08-19 | Cigarette additive extracted from natural plant, and extracting method and use in cigarette thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2006097010A1 (en) * | 2005-03-14 | 2006-09-21 | Xixian Qiu | AN INSTANT ADDITIVE SOLUTION FOR THE FILTER OF CIGARETTl, ITS PRODUCTION METHOD AND USE |
| KR100833652B1 (en) * | 2006-12-28 | 2008-05-29 | 한국화학연구원 | Composition for the prevention or treatment of degenerative brain diseases, including pagoji seed extract that inhibits the activity of BAC-1 or an active substance isolated therefrom |
| CN101669674A (en) * | 2008-09-10 | 2010-03-17 | 江西中烟工业公司 | Pilocarpus plant extract for reducing smoke dry sensation of cigarettes and preparation method thereof |
| CN101863896A (en) * | 2010-06-22 | 2010-10-20 | 浙江大学 | A compound extraction method for extracting coumarin from Baizhi |
| CN102090712A (en) * | 2010-12-29 | 2011-06-15 | 华宝食用香精香料（上海）有限公司 | Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes |
| CN104905405A (en) * | 2015-06-17 | 2015-09-16 | 湖北中烟工业有限责任公司 | Preparation method and application of tobacco tip bar containing plant flavone essence |
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| CN102754911B (en) * | 2012-07-02 | 2015-01-21 | 广西中烟工业有限责任公司 | Harm reducing natural plant additive for cigarettes, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2006097010A1 (en) * | 2005-03-14 | 2006-09-21 | Xixian Qiu | AN INSTANT ADDITIVE SOLUTION FOR THE FILTER OF CIGARETTl, ITS PRODUCTION METHOD AND USE |
| KR100833652B1 (en) * | 2006-12-28 | 2008-05-29 | 한국화학연구원 | Composition for the prevention or treatment of degenerative brain diseases, including pagoji seed extract that inhibits the activity of BAC-1 or an active substance isolated therefrom |
| CN101669674A (en) * | 2008-09-10 | 2010-03-17 | 江西中烟工业公司 | Pilocarpus plant extract for reducing smoke dry sensation of cigarettes and preparation method thereof |
| CN101863896A (en) * | 2010-06-22 | 2010-10-20 | 浙江大学 | A compound extraction method for extracting coumarin from Baizhi |
| CN101863896B (en) * | 2010-06-22 | 2012-07-18 | 浙江大学 | Composite extraction method for extracting coumarin from radix angelicae dahuricae |
| CN102090712A (en) * | 2010-12-29 | 2011-06-15 | 华宝食用香精香料（上海）有限公司 | Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes |
| CN104905405A (en) * | 2015-06-17 | 2015-09-16 | 湖北中烟工业有限责任公司 | Preparation method and application of tobacco tip bar containing plant flavone essence |
| CN104905405B (en) * | 2015-06-17 | 2018-05-25 | 湖北中烟工业有限责任公司 | The cigarette of the essence containing plant flavone mouth stick preparation method and application |
| CN112471590A (en) * | 2020-12-04 | 2021-03-12 | 新火智造(深圳)有限公司 | Environment-friendly wrapping-free heating non-combustion naked cigarette bomb |
| CN112471590B (en) * | 2020-12-04 | 2021-11-02 | 新火智造(深圳)有限公司 | Environment-friendly wrapping-free heating non-combustion naked cigarette bomb |
| WO2022116904A1 (en) * | 2020-12-04 | 2022-06-09 | 新火智造(深圳)有限公司 | Method for manufacturing environment-friendly unwrapped heat-not-burn naked cartridge |
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| CN1225998C (en) | 2005-11-09 |
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Free format text: CORRECT: ADDRESS; FROM: 518102 2/F, BUILDING A, DABAIHUI NEW AND HIGH TECHNOLOGY INDUSTRIAL PARK, SHENYAN ROAD, YANTIAN DISTRICT, SHENZHEN CITY, GUANGDONG PROVINCE TO: 518102 ROOM 1102, 11/F, BUILDING A, DABAIHUI NEW AND HIGH TECHNOLOGY INDUSTRIAL PARK, SHENYAN ROAD, YANTIAN DISTRICT, SHENZHEN CITY, GUANGDONG PROVINCE |
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Effective date of registration: 20110412 Address after: 518102 Guangdong province Shenzhen city road salt Yantian District grand Parkway high tech Industrial Park A building 11 floor, room 1102 Patentee after: SHENZHEN DABAIHUI TECHNOLOGY Co.,Ltd. Address before: 518102 East Shenzhen road salt Yantian District grand Parkway high tech Industrial Park A Building 2 floor Patentee before: GUANGDONG SHENNONG YANKE TECHNOLOGY Co.,Ltd. |
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