CN101928352B - Extraction for active ingredients of cordyceps sinensis and application thereof in cigarette filter - Google Patents
Extraction for active ingredients of cordyceps sinensis and application thereof in cigarette filter Download PDFInfo
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- CN101928352B CN101928352B CN2010102586851A CN201010258685A CN101928352B CN 101928352 B CN101928352 B CN 101928352B CN 2010102586851 A CN2010102586851 A CN 2010102586851A CN 201010258685 A CN201010258685 A CN 201010258685A CN 101928352 B CN101928352 B CN 101928352B
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Abstract
The invention discloses extraction for active ingredients of cordyceps sinensis and application thereof in a cigarette filter, and relates to a method for extracting the active ingredients of the cordyceps sinensis from the active ingredients and adding the active ingredients into the cigarette filter. The method comprises the following steps of: after pre-treating and crushing the cordyceps sinensis, heating and refluxing the crushed cordyceps sinensis with water or ethanol; and concentrating, filtering and separating by column chromatography to obtain the active ingredients. The active ingredients of the cordyceps sinensis are added into materials for making the cigarette filter in proportion; and the cigarette filter is made by using the materials. After adopting the technology, the smoking quality of cigarettes can be improved, the release amount of certain harmful components in the mainstream smoke of the cigarettes can be reduced, the active ingredients of the cordyceps sinensis can be transferred into the mainstream smoke, and the effects of promoting the production of body fluid, wetting whistle, eliminating phlegm, reducing stimulus and the like are achieved without any side effect.
Description
Technical field
A kind of extraction of active ingredients of cordyceps sinensis and the application in cigarette filter thereof relate to and from entomophyte, extract its effective constituent, and add the method in the cigarette filter to.
Background technology
Along with smoking and healthy problem more and more receive publicity, the objectionable constituent of sucking security, increase nourishing function, reducing in the cigarette smoke that improve cigarette are the inevitable development trend of cigarette.Some developed countries of the world have made the restriction of specifically limiting the quantity of to the objectionable constituent burst size of commercial cigarettes in succession; And the enhancing of human consumer's self health and environmental consciousness, the cigarette product of developing the lower harm composition of low tar more and improving the organoleptic quality of cigarette meets the trend of World tobacco.
The adding technique that utilizes cigarette filter is that people are devoted to study one of technological method of taking for head it off in recent years.Like the domestic and international various filter tips such as vinegar fibre, third fibre, compound, cavity, biology that occurred, through unremitting research for many years, filter tip has developed into a kind of important techniques measure of cigarette lowering harm and decreasing coking.Special Cigarette Filter is of a great variety, can be divided into lowering harm and decreasing coking filter tip and perfuming filter tip by effect; Can be divided into two compound and three composite filter tips by structure.
Chinese herbal medicine resource is the great treasure-house that China working people is used for preventing and curing diseases, and theory of traditional Chinese medical science is of extensive knowledge and profound scholarship, and the cultural connotation inside information is deep.Herbal medicine is widely used in fields such as food, daily use chemicals Chemicals at present, at cigarette industry starting is also arranged, and adds herbal medicine and falls the developing direction that harmful composition has become the Chinese style cigarette.We can seek Chinese herbal medicine resource, the burst size of selectivity reducing cigarette fume objectionable constituent in the hope of not influencing the cigarette organoleptic quality from intrinsic advantage.
Entomophyte is one type of crucial medicinal fungi, is to parasitize the entomogenous fungi complex body that fungi and its host insect on the insect body form, and is under the jurisdiction of Ascomycetes (Ascomycetes), Clavicipitaceae (Claricipitaceae), Cordyceps (Cordyceps).Research in recent years shows: entomophyte have calmness, antibacterial, suppress many-sided pharmacological actions such as mouse ascites cancer, enhancing body immunologic function.Entomophyte has various active composition (for example polysaccharide, cordycepic acid, cordycepin and adenosine etc.), and these activeconstituentss have pharmacological action widely.
A large amount of medical experiments confirm, but the Cordyceps Polysaccharide activated macrophage stimulates antibody to produce, and improves body immunity.Cordyceps polysaccharide (CP) is hindered chmice acute chemical liver and is had provide protection, and the experiment of Kiho etc. shows that Cordyceps polysaccharide has the effect of remarkable function of reducing blood sugar bioactivity, the effective constituent of aweto nourishing and nourishing yin effect to diabetic mice.
The entomophyte cordycepin: have antibiotic, anti-inflammatory, anti-oxidant, antitumor, regulate effect such as human endocrine.
Entomophyte adenosine: have the merit of participating in body metabolism and physiological regulation.
Entomophyte cordycepic acid: recent clinical, pharmacological research report; Cordycepic acid can suppress the growth of various germs, can prevent and treat cerebral thrombosis, hematencephalon, myocardial infarction, long-term depleted, and cordycepic acid can be protected lung kidney-nourishing, hemostasis and phlegm; Obviously strengthen segmental bronchus cilia activity ability; Regulate bronchial smooth muscle, and can remove the strongest hydroxy radical qiao of toxicity in the human body, and numerous diseases are had obvious curative effects.This have with entomophyte invigorate the lung and the kidney, hemostasis and phlegm, the effect that improves the health be consistent.
At present both at home and abroad relevant research major side to active ingredients of cordyceps sinensis overweights that structure is identified and at aspect such as medical, not finding has the application precedent in tobacco.
Summary of the invention
The objective of the invention is from entomophyte, to extract its effective constituent, and add in the cigarette filter, to reduce the harm of smoking human body.
The objective of the invention is to realize through following scheme:
(1) entomophyte is being crushed to the 40-100 order after the oven dry down at 30-60 ℃, or under the liquid nitrogen condition, is being crushed to the 40-100 order after washing, removing the processing in early stage of impurity, airing.
(2) under 80-100 ℃ or UW or microwave condition, water or 20-90% alcoholic acid ethanol carry out reflux 1-10h to pulverizing back entomophyte;
(3) behind the filtration under diminished pressure, be 80%, make cordyceps extracting liquid obtaining the content that filtrate decompression is concentrated to dry-matter;
(4) in concentrating feed liquid, add 10 times～40 times 95% ethanol of its volume, under 4 ℃, leave standstill more than the 8h behind the mixing, through centrifugal, filter after, and with promptly obtaining Cordyceps Polysaccharide of the present invention after washing with alcohol, the drying;
(5) merging filtrate and washings; With 20-40% ethanol is moving phase, separates through column chromatography (silicagel column, alumina column or macroporous resin etc. are filler), flows out cordycepic acid, cordycepin, adenosine successively; Concentrate respectively then, can obtain the single active ingredient of entomophyte worm;
The consumption that (6) will prop up with 0.10-20 μ g/ by the cordyceps extracting liquid that (3) obtain adds in the vinegar fibre or the third fine filter tip tackiness agent, in the filter tip production process, adds in the filter tip with the filter tip tackiness agent, processes cigarette filter;
(7) will be through the single active ingredient of separating entomophyte in cordycepic acid: Cordyceps Polysaccharide: adenosine: cordycepin=3: 0.5: 0.01: 0.01 ratio be composite; Behind 30% dissolve with ethanol; Prop up by 0.10-20 μ g/ and to add in the fine or third fine filter tip tackiness agent of vinegar; In the filter tip production process, add in the filter tip with the filter tip tackiness agent, process cigarette filter;
(8) will be through the single active ingredient of separating entomophyte in cordycepic acid: Cordyceps Polysaccharide: adenosine: cordycepin=3: 0.5: 0.01: 0.01 ratio be composite; Behind 30% dissolve with ethanol; Prop up consumption by 0.10-20 μ g/ and add many cavitys materials such as gac, zeolite, silicate or molecular sieve to they are uniformly dispersed on how empty material, then with the compound binary composite filter tip that makes of common filter tip.
With the cordyceps extracting liquid or the Cordyceps Polysaccharide that will obtain in (3) of the present invention: adenosine: cordycepin=3: 0.5: 0.01: the composite effective constituent of 0.01 ratio is added in the filter tip; When burning and sucking cigarette; The flue gas free from extraneous odour, have promote the production of body fluid, wet one's whistle, sharp phlegm and fall the evil effect.Concrete usage ratio is: effective constituent is being the 0.10-20 μ g of filter tip weight.
Substantive features of the present invention be utilize entomophyte to extract liquid concentrator or through the single active ingredient of separating entomophyte in cordycepic acid: Cordyceps Polysaccharide: adenosine: cordycepin=3: 0.5: 0.01: 0.01 ratio is composite; Can selective capture objectionable constituent; These functional ingredient can get in human consumer's the oral cavity with flue gas aerosol simultaneously; Play the effect of gain; Can obviously improve or improve the quality quality of cigarette, have the effect of promoting the production of body fluid significantly and certain relieving cough function, can reduce the burst size of some objectionable constituent in the cigarette mainstream flue gas; And do not change the existing complete processing of cigarette filter, therefore have the meaning and the using value of important actual production.
The present invention compares prior art and has the following advantages:
1. can improve the sucking quality of cigarette;
2. can reduce the burst size of some objectionable constituent in the cigarette mainstream flue gas;
3. active ingredients of cordyceps sinensis is transferred in the main flume;
4. has effects such as promoting the production of body fluid, wet one's whistle, eliminate the phlegm, reduce stimulation;
5. without any side effects.
Through testing: utilize the made filter stick of the present invention, the cigarette of production can make the rate of transform of active ingredients of cordyceps sinensis can reach 5-20%; Compare with the contrast cigarette, the content of some objectionable constituent in the cigarette mainstream flue gas, like flue gas benzopyrene, tobacco-specific nitrosamine, smoke gaseous phase free radical etc., the reduction amplitude is between 20-45%, and especially effect is better aspect reduction cigarette smoke radical; When cigarette burns and sucks, the flue gas free from extraneous odour, have promote the production of body fluid, wet one's whistle, effect such as sharp phlegm.
Embodiment
Embodiment 1:
Get the entomophyte dry product, the water washes clean, pick out impurity after, dry or dry.Dry the back down or under liquid nitrogen, be crushed to the 40-100 order at 50 ℃; Get 1000g entomophyte powder under 90 ℃ of conditions, with water extraction or 20-80% extraction using alcohol entomophyte 7h, with qualitative filter paper suction filtration, filtering residue, extracting solution 600g, repeat to extract twice again, merge the 2000g extracting solution; With the concentrated down 200g liquid concentrator that obtains of extracting solution decompression; Add the extracting solution of the entomophyte that obtains to the filter tip tackiness agent by 0.01% respectively, the functional filter tip of preparation rolls into cigarette finished product.
Embodiment 2:
Get the entomophyte dry product, the water washes clean, pick out impurity after, dry or dry; After oven dry under 50 ℃, be crushed to the 40-100 order; Under 90 ℃ of conditions, with water extraction entomophyte 7h, after the content that filtrate filtered is concentrated to dry-matter is 5%; With the filtrating after concentrating, by filtrating: ethanol is that 1: 3 volume ratio adds absolute ethyl alcohol, under 4 ℃, leaves standstill more than the 8h behind the mixing; Through centrifugal, filter after, washing with alcohol is dissolved in water once more; After utilizing the Sevage method to slough the albumen in the polysaccharide, after drying, promptly get Cordyceps Polysaccharide composition of the present invention.
Merge above-mentioned filtrating and the washing with alcohol liquid of obtaining; Through be concentrated into initial volume 1/10 after, through column chromatography (silica gel, aluminum oxide or macroporous resin are stopping composition), be moving phase with 20-40% ethanol; Utilize thin-layer chromatography to be monitoring means; Separating effective ingredient through concentrating under reduced pressure, separates obtaining effective active compositions such as corresponding entomophyte cordycepic acid, cordycepin, adenosine respectively.
Embodiment 3:
A kind of binary composite filter tip of forming a kind of harm reduction gain by common filter stick and functional filter stick.How empty materials such as gac, zeolite are immersed in the extraction enriching soln of 5% Cordyceps Polysaccharide, make it to be uniformly dispersed, obtain functional sorbent material after the drying.This functional sorbent material is being added on the filter-stick forming device on the fibrous bundle of shredding equably; Process the function filter stick; The weight percent of function property sorbent material and functional filter stick is 30%; To make the function filter stick and common filter stick makes the binary composite filter tip, be a kind of composite filter tip of effective harm reduction gain.
Embodiment 4:
A kind of binary composite filter tip of forming a kind of harm reduction gain by common filter stick and functional filter stick.With cordycepic acid: Cordyceps Polysaccharide: adenosine: cordycepin=3: 0.5: 0.01: 0.01 ratio is composite; Be mixed with 0.2% ethanolic soln; How empty materials such as gac, zeolite are immersed in this ethanolic soln, make it to be uniformly dispersed, obtain functional sorbent material after the drying.This functional sorbent material is being added on the fibrous bundle of shredding on the filter-stick forming device equably, is processing the function filter stick, controlling that effective constituent can be 0.10-20 μ g in every cigarette filter tip.To make the function filter stick and common filter stick makes the binary composite filter tip, be a kind of composite filter tip of effective harm reduction gain.
Claims (4)
1. the process for extracting of an active ingredients of cordyceps sinensis is characterized in that the process for extracting of active ingredients of cordyceps sinensis is:
A. entomophyte is being crushed to the 40-100 order after the oven dry down at 30-60 ℃, or under the liquid nitrogen condition, is being crushed to the 40-100 order after washing, removing the processing in early stage of impurity, airing;
B. under 80-100 ℃ or UW or microwave condition, the ethanol of water or 20-90% carries out reflux 1-10h to pulverizing back entomophyte;
C. behind the filtration under diminished pressure, be 80%, make cordyceps extracting liquid obtaining the content that filtrate decompression is concentrated to dry-matter;
D. in concentrating feed liquid, add 10 times～40 times 95% ethanol of its volume, under 4 ℃, leave standstill more than the 8h behind the mixing, through centrifugal, filter after, and with promptly obtaining Cordyceps Polysaccharide after washing with alcohol, the drying;
E. merging filtrate and washings; With 20-40% ethanol is moving phase, is the column chromatography for separation of filler through silicagel column, alumina column or macroporous resin, flows out cordycepic acid, cordycepin, adenosine successively; Concentrate respectively then, can obtain the single active ingredient of entomophyte.
2. method according to claim 1 is extracted the application of active ingredients of cordyceps sinensis in cigarette filter that obtains; It is characterized in that the consumption that cordyceps extracting liquid props up with 0.10-20 μ g/ is added in the vinegar fibre or the third fine filter tip tackiness agent; In the filter tip production process; Add in the filter tip with the filter tip tackiness agent, process cigarette filter.
3. method according to claim 1 is extracted the application of active ingredients of cordyceps sinensis in cigarette filter that obtains; It is characterized in that will be through the single active ingredient of separating entomophyte in cordycepic acid: Cordyceps Polysaccharide: adenosine: cordycepin=3: 0.5: 0.01: 0.01 ratio is composite; Behind 30% dissolve with ethanol, prop up by 0.10-20 μ g/ and to add in the fine or third fine filter tip tackiness agent of vinegar, in the filter tip production process; In filter tip, process cigarette filter with the filter tip tackiness agent.
4. method according to claim 1 is extracted the application of active ingredients of cordyceps sinensis in cigarette filter that obtains; It is characterized in that will be through the single active ingredient of separating entomophyte in cordycepic acid: Cordyceps Polysaccharide: adenosine: cordycepin=3: 0.5: 0.01: 0.01 ratio is composite; Behind 30% dissolve with ethanol; Prop up consumption by 0.10-20 μ g/ and add gac, zeolite, silicate or molecular sieve to they are uniformly dispersed on how empty material, then with the compound binary composite filter tip that makes of common filter tip.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102586851A CN101928352B (en) | 2010-08-13 | 2010-08-13 | Extraction for active ingredients of cordyceps sinensis and application thereof in cigarette filter |
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| CN2010102586851A CN101928352B (en) | 2010-08-13 | 2010-08-13 | Extraction for active ingredients of cordyceps sinensis and application thereof in cigarette filter |
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| CN101928352B true CN101928352B (en) | 2012-06-06 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103113442B (en) * | 2013-02-28 | 2015-04-22 | 华南理工大学 | Method for extracting cordyceps polysaccharide and adenosine from cordyceps sinensis mycelium |
| CN103238701A (en) * | 2013-05-23 | 2013-08-14 | 昆明宝特药用植物研究开发有限公司 | Food composition applicable to smoking and drinking crowds and preparation method of food composition |
| CN103435712A (en) * | 2013-08-27 | 2013-12-11 | 王辉 | Extraction method of cordyceps sinensis intracellular polysaccharide |
| CN103494845A (en) * | 2013-09-30 | 2014-01-08 | 涂峰 | Production method of hirsutella sinensis hypha extract |
| CN103549658A (en) * | 2013-11-14 | 2014-02-05 | 上海国宝企业发展中心 | Method for reducing harmful substances in cigarette with main active substances in cordyceps militaris and product |
| CN105011350A (en) * | 2014-04-30 | 2015-11-04 | 上海绿馨电子科技有限公司 | Electronic cigarette oil containing cordyceps and preparation method thereof |
| CN107556358B (en) * | 2017-09-27 | 2019-08-23 | 黄河科技学院 | Promote blood coagulation Cordyceps militaris effective component and its purification methods and uses |
| CN109953365A (en) * | 2019-03-22 | 2019-07-02 | 内蒙古昆明卷烟有限责任公司 | A kind of preparation method and application of cordyceps extracting liquid |
| CN109953366B (en) * | 2019-03-22 | 2022-11-11 | 内蒙古昆明卷烟有限责任公司 | Cordyceps sinensis extracting solution and preparation method, composition and application thereof |
| CN110256591B (en) * | 2019-06-21 | 2022-02-15 | 东莞市东阳光冬虫夏草研发有限公司 | Cordyceps sinensis polysaccharide extract and preparation method and application thereof |
| CN112980574A (en) * | 2021-01-20 | 2021-06-18 | 广东澳大新化工有限公司 | Glycerol triacetate reactant of cordyceps sinensis and application of glycerol triacetate reactant in cigarettes |
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| CN101015571B (en) * | 2007-03-13 | 2010-09-08 | 陈林生 | Chinese caterpillar fungus polysaccharide buccal tablets and its preparing process |
| CN101229199B (en) * | 2008-01-15 | 2010-06-02 | 重庆和润生物工程有限公司 | Integrative extract method of multi-active ingredient in cordyceps militaris mycelium |
| CN101508715B (en) * | 2009-04-01 | 2011-05-04 | 江苏省农业科学院 | Extraction and purification process for cordycepin in cordyceps militaris link |
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