CN102987548B - Plant extract capable of reducing harmful substances in cigarette and preparation method thereof - Google Patents
Plant extract capable of reducing harmful substances in cigarette and preparation method thereof Download PDFInfo
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- CN102987548B CN102987548B CN201210515417.2A CN201210515417A CN102987548B CN 102987548 B CN102987548 B CN 102987548B CN 201210515417 A CN201210515417 A CN 201210515417A CN 102987548 B CN102987548 B CN 102987548B
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Abstract
The invention belongs to the technical field of cigarette tar and harmful substance reduction and particularly relates to a plant extract capable of reducing the harmful substances in the cigarette and a preparation method thereof, aiming to achieve the purpose of reducing the content of NH3 in the main stream smoke effectively. According to the technical scheme for solving the problems in the prior art, the method for preparing the plant extract comprises the following steps: (1) preparing a volatile extract, (2) preparing a non-volatile extract, and (3) mixing. The plant extract provided by the invention is a natural pure Chinese medicine and is added into the cigarette according to a certain proportion after being purified by adopting the precise purification process so that the NH3 generated from the combustion of the cigarette is reduced effectively.
Description
Technical field
The invention belongs to Tar technical field, be specifically related to a kind of plant extraction liquid that can reduce the harmful substance in cigarette and preparation method thereof.
Background technology
" Framework Convention on Tobacco Control " sign with come into force after, State Tobacco Monopoly Bureau has organized the research work of cigarette harmfulness index, choose domestic 163 kinds of main representative cigarette brands (specification), the main Huffman analyte of research cigarette mainstream flue gas burst size and the dependency relation of recommending in the world 3 flue gas toxicologic index, the acute lethal test of animal.Result of study shows, CO, HCN, NNK, NH3, benzo [a] pyrene, phenol, 7 kinds of harmful components burst sizes of crotonaldehyde can Efficient Characterization cigarette mainstream flue gas biohazardous, although the overall releasing content of coke tar of Chinese style flue-cured tobacco type cigarette is higher than external blended type cigarette, but flue gas bio-toxicity and external blended type cigarette no significant difference, part harmful components (as NNK) are even lower than external blended type cigarette.
There are abundant natural plant resource and extensive traditional Chinese medical theory in China, and natural plants, for cigarette, can effectively be reduced to main flume harmful components and hazard index, improves Product Safety, enriches cigarette flavor style.The harm reduction of application Chinese herbal medicine, flavouring, be to meet the exploitation " Chinese-style cigarette " that State Bureau advocates, and walks " evil falls in green " with Chinese characteristics road.
Summary of the invention
The object of this invention is to provide a kind of plant extraction liquid that can reduce the harmful substance in cigarette and preparation method thereof, to reach the object of the content of NH3 in effective reduction main flume.
The problem existing for solving prior art, technical scheme provided by the invention is:
The preparation method that can reduce the plant extraction liquid of the harmful substance in cigarette, is characterized in that: comprises the following steps,
One, volatile extract preparation:
1) raspberry 1000g is dried 3 hours at 105 DEG C, pulverize, cross 100 mesh sieve screenings;
2) pulverize rear sample and adopt benzinum to carry out lixiviate 3 times, reclaim solvent and obtain 150 grams of medicinal extract extracts;
3) adopt absolute alcohol to dissolve, under condition of normal pressure, 0 DEG C leaves standstill about 12 hours, filters, and recovered alcohol, obtains 80 grams of volatile extracts;
Two, non-volatile extract preparation:
1) raspberry 1000g is dried 3 hours at 105 DEG C, pulverize, cross 100 mesh sieve screenings;
2) pulverize rear sample and adopt benzinum to carry out lixiviate 3 times, after filtration, obtain 850 grams of the dregs of a decoction;
3) adopt aqueous extraction-alcohol precipitation technology, filtering-depositing reclaims solvent to dry 200 ~ 300 grams of the extracts that obtain;
4) refining: the product of step 3) is further purified and obtains 120 ~ 150 grams of refining extracts through resin.
Three, compatibility:
The extract of the extract of step 1 and step 2 is carried out to compatibility according to the ratio of 1:2, after solvent allotment, obtain final plant extraction liquid.
In above-mentioned steps two the 3rd) technological parameter in the aqueous extraction-alcohol precipitation technology of step is respectively: add the water of 12 times of dregs of a decoction volume, decoct 3 times, decoct 1h at every turn, alcohol precipitation concentration is 80%, and crude drug concentration is 1.0:1.0.
In above-mentioned steps two the 4th) resin of step is AB-8 type macroreticular resin.
The plant extraction liquid that utilizes the preparation method of the above-mentioned plant extraction liquid that can reduce the harmful substance in cigarette to prepare.
The present invention is with respect to prior art, and tool has the following advantages and effect:
Plant extraction liquid of the present invention is natural pure Chinese medicine, carries after technique is purified and adding to by a certain percentage in cigarette through essence, can effectively suppress to reduce the generation of NH3 in combustion process.
Brief description of the drawings
Fig. 1 is that additive extracts purifying flow chart;
Fig. 2 is volatile extract total ion current figure;
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is elaborated:
With reference to Fig. 1, a kind of preparation method of the plant extraction liquid that can reduce the harmful substance in cigarette, comprises the following steps:
One, volatile extract preparation (route one, Fig. 1 left side)
Raspberry 1000g is dried 3 hours at 105 DEG C, pulverize, cross 100 mesh sieve screenings, after pulverizing, sample adopts benzinum to carry out lixiviate 3 times, reclaims solvent and obtains 150 grams of medicinal extract extracts, adopts absolute alcohol to dissolve, under condition of normal pressure, 0 DEG C leaves standstill about 12 hours, filter, recovered alcohol, obtains 80 grams of volatile extracts; This route is mainly the composition such as fat-soluble pigment, LCFA of removing in extract, to reduce, cigarette flavor is produced to harmful effect.
With reference to Fig. 2, adopt GC-MS to analyze volatile ingredient, ensure the controllability of the quality of volatile extract.
Two, non-volatile extract preparation (route two, Fig. 1 right side)
Raspberry 1000g dries 3 hours at 105 DEG C, pulverizes, and crosses 100 mesh sieve screenings, and after pulverizing, sample adopts benzinum to carry out lixiviate 3 times.After filtration, obtain 850 grams of the dregs of a decoction, adopt aqueous extraction-alcohol precipitation technology, filtering-depositing reclaims solvent to dry 200 ~ 300 grams of the extracts that obtain.Then be further purified and obtain 120 ~ 150 grams of refining extracts through resin, this route is mainly to remove polysaccharide, nucleic acid in extract, and the macromolecular substances such as protein, water colo(u)r, produce harmful effect to reduce to cigarette flavor.
Choosing of aqueous extraction-alcohol precipitation technology parameter:
Chinese medicine dreg after benzinum is extracted adopts water extract-alcohol precipitation method, taking ellagic acid as index optimization extraction process, alcohol adding amount and determining alcohol in the factors such as amount of water, decocting time and the decoction number of times in employing orthogonal experiment Optimization Analysis decocting process and alcohol precipitation process.
Orthogonal Experiment and Design: the amount of water (A) to medicinal material, decocting time (B), 3 factors of decoction number of times (C) are investigated. determine the optimum condition of extraction process.Orthogonal test factor level is in table 1.
From table 2, adopt HPLC to detect, taking ellagic acid content (mg/g), during as index, the order that affects its result is C>A> B.As can be seen here. extraction time has the greatest impact, and amount of water takes second place, and extraction time is minimum on its impact, and optimised process is A2B2C3; During taking total extract as index, the order that affects its result is C> B>A, and extraction time has the greatest impact to it, and extraction time takes second place, amount of water is minimum on its impact, optimised process is A2B3C3, has reached good effect but extract 1.0h, and comprehensive production cost is considered, so determine that extraction time is 1.0h, ellagic acid optimum extraction process is A2B2C3, adds 12 times of water gagings of volume ratio, extracts 3 times. extract 1.0h at every turn.
Alcohol precipitation process parameter is chosen:
Because total extract contains more impurity, after burning, can cause harmful effect to cigarette smoke, in order to reduce cigarette foreign gas and to improve polyphenol compound content, need to take alcohol precipitation process to its purifying.Take 120g raw material, extract according to optimised process, extract mixes, and is divided into 12 equal portions, is concentrated into respectively crude drug amount and medicine liquid volume than being each 6 parts of 1.0:1.0 and 1.2:1.Every 2 parts 1 group, 3 groups of each density are sink to 60%, 70% with ethanol alcohol respectively, and 80% filters, and place 12 h and carry out ellagic acid assay and alcohol precipitation total extract mensuration, the results are shown in Table 3.
From alcohol precipitation result of the test, under same density, along with increasing of alcohol precipitation concentration, ellagic acid content constantly increases, and total extract reduces gradually, is 80% therefore select alcohol precipitation concentration.And for different densities, be concentrated into 1.0:1.0 and be concentrated into 1.0:1.2, ellagic acid content and total extract all reduce to some extent, but without significant change.Consider ellagic acid content and ethanol cost and concentration time. intending adopting crude drug concentration is that 1.0:1.0 carries out alcohol precipitation.
Choosing of refining resin:
In order further to remove impurity, water extract-alcohol precipitation liquid is divided into 4 parts, add respectively the macroporous absorbent resin (D-101 of 4 kinds of models, AB-8, HPD-400, NKA-II) in, water and 70% ethanol carry out wash-out successively, the recovery rate (after desorb in the front extract of the ellagic acid content of gained and upper prop the ratio of ellagic acid content) that calculates ellagic acid, experimental result is as follows:
From above-mentioned result of the test, AB-8 macroreticular resin separation and purification ellagic acid recovery rate is higher, selects AB-8 type macroreticular resin therefore definite.
3, compatibility
Prepare volatile extract and the water extract-alcohol precipitation extract two parts containing ellagic acid according to above-mentioned process route, for falling of complete embodiment additive is harmful, cause fragrant effect, volatile extract and water extract-alcohol precipitation extract two parts extract are carried out to compatibility according to the ratio of 1:2 left and right, after solvent allotment for Harm reduction techniques blending.
Two, the application in cigarette
1, control sample is reinforced applies according to 3.0% pure water, and perfuming applies according to 0.7% alcohol (75%).
2, raspberry extract is reinforced applies in 2.0% ratio, and perfuming applies according to 1.0% ratio.
Three, effect assessment
1, harm reduction effect
The sample of preparation is added in Virginian-type cigarette tobacco leaf formulation in reinforced, perfuming step with 2% and 1% consumption respectively, seven Harmful ingredient contents are detected after rolling packaging, fall harmful effect and see the following form.
2, the impact on cigarette quality
。
Claims (4)
1. the preparation method that can reduce the plant extraction liquid of the harmful substance in cigarette, is characterized in that: comprises the following steps,
One, volatile extract preparation:
1) raspberry 1000g is dried 3 hours at 105 DEG C, pulverize, cross 100 mesh sieve screenings;
2) pulverize rear sample and adopt benzinum to carry out lixiviate 3 times, reclaim solvent and obtain 150 grams of medicinal extract extracts;
3) adopt absolute alcohol to dissolve, under condition of normal pressure, 0 DEG C leaves standstill 12 hours, filters, and recovered alcohol, obtains 80 grams of volatile extracts;
Two, non-volatile extract preparation:
1) raspberry 1000g is dried 3 hours at 105 DEG C, pulverize, cross 100 mesh sieve screenings;
2) pulverize rear sample and adopt benzinum to carry out lixiviate 3 times, after filtration, obtain 850 grams of the dregs of a decoction;
3) adopt aqueous extraction-alcohol precipitation technology, filtering-depositing reclaims solvent to dry 200 ~ 300 grams of the extracts that obtain;
4) refining: the product of step 3) is further purified and obtains 120 ~ 150 grams of refining extracts through resin;
Three, compatibility:
The extract of the extract of step 1 and step 2 is carried out to compatibility according to the ratio of 1:2, after solvent allotment, obtain final plant extraction liquid.
2. can reduce according to claim 1 the preparation method of the plant extraction liquid of the harmful substance in cigarette, it is characterized in that: in described step 2 the 3rd) technological parameter in the aqueous extraction-alcohol precipitation technology of step is respectively: the water that adds 12 times of amounts of dregs of a decoction volume, decoct 3 times, each 1h that decocts, alcohol precipitation concentration is 80%, and medicine liquid volume is than being 1.0:1.0.
3. according to the preparation method that can reduce the plant extraction liquid of the harmful substance in cigarette described in claim 1 or 2, it is characterized in that: in described step 2 the 4th) resin of step is AB-8 type macroreticular resin.
4. a plant extraction liquid that utilizes the preparation method of the plant extraction liquid that can reduce the harmful substance in cigarette described in claim 1 to prepare.
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| CN102987548B true CN102987548B (en) | 2014-09-17 |
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Families Citing this family (2)
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| CN104207325A (en) * | 2013-05-29 | 2014-12-17 | 王天华 | Application of blackberry extractives in cigarettes |
| CN104207326A (en) * | 2013-05-29 | 2014-12-17 | 王天华 | Application of raspberry extract in cigarette |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1530421A (en) * | 1975-03-11 | 1978-11-01 | Givaudan & Cie Sa | Odorants and/or flavourants containing theaspiran |
| CN101732440A (en) * | 2009-12-15 | 2010-06-16 | 中国人民解放军第二军医大学 | Raspberry extract and raspberry element obtain by separation thereof and application thereof |
| CN101804127A (en) * | 2010-04-28 | 2010-08-18 | 北京大学第一医院 | Compound traditional Chinese medicine extractive composite for preventing and curing Alzheimer disease |
| CN102599652A (en) * | 2011-01-20 | 2012-07-25 | 梁永林 | Cigarette filter for inhibiting nicotine addiction |
-
2012
- 2012-12-05 CN CN201210515417.2A patent/CN102987548B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1530421A (en) * | 1975-03-11 | 1978-11-01 | Givaudan & Cie Sa | Odorants and/or flavourants containing theaspiran |
| CN101732440A (en) * | 2009-12-15 | 2010-06-16 | 中国人民解放军第二军医大学 | Raspberry extract and raspberry element obtain by separation thereof and application thereof |
| CN101804127A (en) * | 2010-04-28 | 2010-08-18 | 北京大学第一医院 | Compound traditional Chinese medicine extractive composite for preventing and curing Alzheimer disease |
| CN102599652A (en) * | 2011-01-20 | 2012-07-25 | 梁永林 | Cigarette filter for inhibiting nicotine addiction |
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