CN104087421A - Althaea rosea flower extract coproduction preparation method and applications thereof - Google Patents
Althaea rosea flower extract coproduction preparation method and applications thereof Download PDFInfo
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- CN104087421A CN104087421A CN201410353130.3A CN201410353130A CN104087421A CN 104087421 A CN104087421 A CN 104087421A CN 201410353130 A CN201410353130 A CN 201410353130A CN 104087421 A CN104087421 A CN 104087421A
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Abstract
The invention discloses an althaea rosea flower extract coproduction preparation method. By taking althaea rosea flowers as raw materials, two tobacco flavors are prepared step by step from the same batch of raw material, wherein the preparation steps include extraction and separation. The preparation method particularly comprises the following steps: a. removing impurities from the dried althaea rosea flowers and crushing; b. extracting and concentrating with ethanol to obtain ethanol extract of althaea rosea flower; c. extracting the alcohol-extracted residues by using ammonium water solution; and d. cooling, regulating pH value with hydrochloric acid, and adding an enzyme preparation for conducting constant-temperature reaction; and conducting heating digestion and reduced-pressure concentration to obtain aqueous extract concentrated liquor of althaea rosea flower. The preparation method is mostly characterized in that the two novel tobacco flavors (alcohol extract of althaea rosea flower and aqueous extract concentrated liquor of althaea rosea flower) can be prepared from the althaea rosea flower, the applications of the two flavors cannot change the original performance and processing technology of cigarettes, the flavor quality of the cigarettes can be improved, and the sensation comfortableness of the cigarettes in smoking can be increased; the althaea rosea is widely distributed in China and is abundant, the production technology is simple and easy to operate, the production cost is low, and therefore the althaea rosea flower extract coproduction preparation method has practical production significance and values.
Description
Technical field
The present invention relates to the tobacco aromatics using field in cigaret additive, particularly a kind of Flower of Hollyhock extract co-production preparation method and the application of extract in cigarette thereof.The enforcement of this technology does not change the existing complete processing of cigarette, can improve suction quality and the sense organ comfort level of cigarette.
Background technology
Along with the tar content of domestic cigarette product constantly reduces, the problems such as the decline of cigarette flavor amount, style and features reduction, comfortableness variation have been caused to some extent.For improving the overall quality of cigarette product, the Novel tobacco flavor of exploitation bright characteristic, stay in grade is a main solution route.This wherein, natural perfume becomes the emphasis of recent researches exploitation because of advantages such as its note is abundant, fragrance is true to nature, safety and environmental protections.
Vast territory and abundant resources in China, and floristics is various, and the composition of contained effective constituent also respectively has feature, for the exploitation of natural perfume provides rich in natural resources.Can to effective ingredients in plant, extract separation by different modes method, and for the feature of cigarette product, extract is applied in cigarette with multi-form, to improving the overall quality of cigarette.
Hollyhock (Althaea rosea(Linn.) Cavan) have another name called that one zhang red, waste of flax is magnificent, chessboard is magnificent, cape is colored, the Dragon Boat Festival is colored, English name hollyhock, the biennial upright herbaceous plant (Feng Guomei of Malvaceae Althaea, Chinese Plants will (the 49th volume the second fascicle, editorial board of Chinese Academy of Sciences's " Chinese Plants will ", Science Press: Beijing, 1984, p11).Hollyhock originates in Southwestern China area, is the plant that the various value such as a kind ofly has ecology, views and admires, eat, be medicinal, extensively cultivate throughout the country Rao Lulu. the hollyhock of many economic uses [J]. vegetables, 2004, (1): 38.}.Hollyhock is used as medicine with root, leaf, flower, seed, and its main medicinal part is the flower of plant, Flower of Hollyhock be the conventional herbal medicine of the ethnic minoritys such as Uygur, Mongolia Liu Yongmin. Uygur medicine will (first volume) [M]. Xinjiang science and technology health press: Urumchi, 1993; The precious sound figure of pp 372-373.; Bu E; Zhao is at the age of one hundred years old. and anaesthetic accounts for the herbal textual [J] of bar. Chinese medicinal materials, 2003,26 (2): 119-120.}.The pigment of Flower of Hollyhock can be used as the tinting material of beverage or food, and tender leaf, petal be edible also.
Flower of Hollyhock contains various active composition, mainly contains flavonoid, organic acid, acidic polysaccharose, pectin and natural plant pigment etc.Flower of Hollyhock flavones content is abundant, is mainly kaempferol, Quercetin, astragalin etc., all has good removing free radical, anti-oxidant, antibacterial effect; Its polysaccharide and pectin are formed by multiple monose or uronic acid bonding, be mainly rhamnosyl, pectinose, semi-lactosi and galacturonic acid, glucuronic acid etc., polysaccharide and pectin can react in the processing of cigarette with in burning and sucking process with other composition in tobacco leaf and produce abundant fragrance matter after degraded; Organic acid can be adjusted flue gas potential of hydrogen when cigarette burns and sucks, and improves cigarette smoking mouthfeel.
Hollyhock is widely distributed in China, and its florescence is long, and aboundresources is cheap.At present, in fields such as medicine, healthcare products and food, there is more applied research, there is not yet the application of its extract in tobacco.
Summary of the invention
The present invention is studied the extracting method of Flower of Hollyhock based on above-mentioned present Research just, adopt suitable extraction, separation means, utilization is prepared two kinds of tobacco aromatics using products step by step with a collection of raw material: Flower of Hollyhock alcohol extract and water extracting liquid, object is to improve suction quality and the sense organ comfort level of cigarette product.
The object of the invention is to be achieved through the following technical solutions:
A Flower of Hollyhock extract co-production preparation method, take Flower of Hollyhock as raw material, adopts extraction, separation means, utilizes and prepares step by step two kinds of tobacco aromatics using products with a collection of raw material, and concrete technology step is as follows:
A. by dry Flower of Hollyhock, removal of impurities, pulverizing;
B. with certain density extraction using alcohol, the concentrated Flower of Hollyhock alcohol extract that to obtain;
C. the material slag after alcohol extracting adds a certain amount of ammonia soln heating to extract;
D. being cooled to after room temperature, is 3.5～5.0 with salt acid for adjusting pH value, adds a certain amount of zymin isothermal reaction for some time; Reheat lixiviate, after vat liquor concentrating under reduced pressure, obtain Flower of Hollyhock water extracting liquid.
In the step b of aforesaid method, during extraction using alcohol, alcohol concn is 60 %～90 %(
v/
v, lower same), feed liquid mass ratio is 1:5～1:15, is heated to 60～85 ℃ and extracts 1～2 time, each 1～3 hour; Extracting solution is 10～50 % through being evaporated to paste containing amount.
In the step c of aforesaid method, ammonia concn used is 0.5 %～1.0 %, and add-on is 6～10 times of Flower of Hollyhock dry powder quality, and under 80～100 ℃ of conditions, heating is extracted 2～3 hours.
In the steps d of aforesaid method, the zymin adding is cellulase and polygalacturonase, and addition is respectively 0.1～0.5 % and 0.5～1.0 % of Flower of Hollyhock dry powder quality, and temperature constant temperature within the scope of 40～55 ℃ is set, enzymolysis time 1～3 hour; Enzyme digestion reaction post-heating to 80～100 ℃ further lixiviate 2～4 hours; Solid-liquid separation afterwards, gained clear liquid is 10～30 % through being evaporated to paste containing amount.
In the step c of aforesaid method, use ammonia soln can effectively extract organic acid and acidic polysaccharose that Flower of Hollyhock contains.In steps d, add the macromole fibrous matter in cellulase degradable cell walls, contribute to the stripping of the effective constituent in born of the same parents; The pectin degrading that polygalacturonase can make to be insoluble in water is reducing sugar.In addition, the small molecular sugar compounds producing in enzymolysis process and micromolecular nitrogenous compound can further generate nitrogen heterocyclic or oxa-lopps material by Maillard reaction again in heat-processed, thereby increase the content of fragrance matter in water extraction liquid, and enrich the note of water extraction liquid, the organoleptic quality of cigarette is had to better improvement effect.Finally heat lixiviate and can reach three objects simultaneously: (1) make zymin deactivation; (2) improve extracting efficiency; (3) thermal response produces fragrance matter.
The Flower of Hollyhock alcohol extract of the inventive method gained is black purple fluid extract, is rich in the aroma component of flavones ingredient and medium and small polarity, has the fragrant and sweet and fragrance of a flower fragrance of the cream of pleasant; After ethanol and/or propylene glycol dilution, add in cigarette, can increase Hui Tian, enrich note, reduce assorted gas, reduce the pungency of cigarette.Concrete usage ratio is tobacco quality 0.01 ‰～0.1 ‰, can be used alone or is deployed into essence with other spices and use.
Flower of Hollyhock water extracting liquid is lavender liquid, after water dilution, with feed liquid, is applied on cigarette shreds, and while burning and sucking cigarette, flue gas free from extraneous odour, can enrichment flue gas, improve fragrance matter, increase sweet sense, reduce dry sensation, improves oral cavity comfortableness.Flower of Hollyhock water extracting liquid consumption is tobacco quality 0.01 ‰～0.5 ‰, can be deployed into essence according to cigarette style and other spices and use.
Maximum feature of the present invention is: provide and take " Flower of Hollyhock alcohol extract " and " Flower of Hollyhock water extracting liquid " two kinds of Novel tobacco flavors that Flower of Hollyhock prepared as raw material, the application of this spices does not all change original performance and the complete processing of cigarette, improved the flavouring essence quality of cigarette, improved sense organ comfort level when cigarette burns and sucks, without any side effects; And hollyhock is widely distributed in China, aboundresources, and production technique is simple to operation, and production cost is lower, therefore have more the meaning and value of actual production.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but do not limit the present invention.
embodiment 1
Get dry Flower of Hollyhock, after removal of impurities, pulverizing, weigh; The 90 % ethanol that add its 12 times of quality, are heated to 70 ℃ and extract 3 hours, treat that feed liquid is cooled to room temperature, and with 400 order filter-cloth filterings, clear liquid is evaporated to paste containing amount 50 % and obtains Flower of Hollyhock alcohol extract.To add in the material slag after alcohol extracting 8 times of Flower of Hollyhock dry powder quality, concentration is the ammonia soln of 1.0 %, in 80 ℃ of heating, extract 3 hours; Being cooled to salt adding acid for adjusting pH value after room temperature is 4.5, adds the cellulase of Flower of Hollyhock dry powder quality 0.2 % and the polygalacturonase of 0.8 %, 40 ℃ of constant temperature 3 hours; Reheat and be warming up to 85 ℃ of backflows 3 hours, stop, after heating, treating that feed liquid is cooled to room temperature, centrifugal 40 min of 4000 rmp, gained clear liquid obtains Flower of Hollyhock water extracting liquid through being evaporated to paste containing amount 10 %.
Take the above-mentioned Flower of Hollyhock alcohol extract of 0.010 g, with 80 % ethanol (also can be propylene glycol), be diluted to 1.000 g, mix, adopting perfuming cigarette injector is 0.05 ‰ to injecting 4 μ L(perfuming amounts in every blank cigarette), be designated as test cigarette 1..Separately get the blank cigarette of part, inject 4 μ L 80 % ethanol (also can be propylene glycol) cigarette in contrast for every.Take again 0.020 g Flower of Hollyhock water extracting liquid, add distilled water to 5.000 g, mix and with micro sprayer, spray equably and be added on the blank pipe tobaccos of 100 g (feeding quantity is 0.2 ‰) afterwards.Pipe tobacco is packed in sealing bag, place 80 ℃ of constant temperature 30 min in baking oven, then shake rapidly pipe tobacco, moisture in cut tobacco is controlled at 12 % left and right, rolls into cigarette, is denoted as test cigarette 2..Two kinds of test cigarette and contrast cigarette are put into respectively to constant temperature (22 ± 1 ℃), constant humidity (relative humidity 60 ± 2 %) case inner equilibrium more than 48 hours.Through the above judging panel of 7 people, smoke panel test, result shows: with contrast cigarette comparison, the cigarette that 1. adds Flower of Hollyhock alcohol extract returns sweet sense to be increased, flue gas appears the fragrance of a flower, delicate fragrance, note is abundanter, assorted gas, stimulation alleviate; Cigarette flavor matter and the perfume quantity of 2. adding Flower of Hollyhock water extracting liquid all have lifting, and pleasant impression is clean, and dry sensation and pungency reduce.The application of two kinds of novel fragrances all can significantly improve the suction quality of cigarette.
embodiment 2
Get dry Flower of Hollyhock, after removal of impurities, pulverizing, weigh; With 80 ℃ of 80 % ethanol, extract 2 times, feed liquid mass ratio is followed successively by 1:7 and 1:6, each 2 hours extraction times, merge extracted twice liquid, and be evaporated to paste containing amount 30 % and obtain Flower of Hollyhock alcohol extract.To add in the material slag after alcohol extracting 10 times of Flower of Hollyhock dry powder quality, concentration is the ammonia soln of 0.5 %, in 90 ℃ of heating, extract 2 hours; Be cooled to after room temperature, salt adding acid for adjusting pH value is 4.0; Add again the cellulase of Flower of Hollyhock dry powder quality 0.5 % and the polygalacturonase of 0.5 %, in 50 ℃ of isothermal reactions 4 hours; Reheat and be warming up to 95 ℃ of backflows 2 hours.Stop, after heating, treating that feed liquid is cooled to room temperature, decompress filter, vacuum tightness-0.08 MPa, gained clear liquid obtains Flower of Hollyhock water extracting liquid through being evaporated to paste containing amount 30 %.
Take the above-mentioned Flower of Hollyhock alcohol extract of 0.100 g, with the mixed solvent of 95 % ethanol and propylene glycol (mass ratio 1:1), be diluted to 10.000 g, mix, standby.Get the pipe tobacco of two parts of even equivalent, portion evenly sprays the diluting soln (perfuming amount is 0.03 ‰) of Flower of Hollyhock alcohol extract by 3 ‰ of pipe tobacco weight on pipe tobacco; Another part pressed mixed solvent that 3 ‰ of pipe tobacco weight evenly sprays 95 % ethanol and propylene glycol (mass ratio 1:1) pipe tobacco in contrast.Then, roll into respectively cigarette.Test cigarette and contrast cigarette are put into respectively to constant temperature (22 ± 1 ℃), constant humidity (relative humidity 60 ± 2 %) more than case inner equilibrium 48 h.Through the above judging panel of 7 people, smoke panel test, result shows: the cigarette that applies Flower of Hollyhock alcohol extract with contrast cigarette comparison, perfume quantity increases, fragrance coordination, mix gas and pungency alleviate, pleasant impression returns sweet comfortable.
Separately take 0.100 g Flower of Hollyhock water extracting liquid, with distilled water diluting to 10.000 g, mix.Get the pipe tobacco of two parts of even equivalent, a diluting soln (perfuming amount is 0.1 ‰) of Flower of Hollyhock water extracting liquid that evenly sprays by 1 % of pipe tobacco weight on pipe tobacco; The distilled water of another part of even sprinkling pipe tobacco weight 1 % is pipe tobacco in contrast.After baking, roll into respectively cigarette.Test cigarette and contrast cigarette are put into respectively to constant temperature (22 ± 1 ℃), constant humidity (relative humidity 60 ± 2 %) more than case inner equilibrium 48 h.Smoking result shows: add the cigarette of Flower of Hollyhock water extracting liquid, and flue gas free from extraneous odour, fragrance matter and perfume quantity all have lifting, and dry sensation and pungency reduce, and Hui Tian promotes the production of body fluid sense obviously.
Claims (6)
1. a Flower of Hollyhock extract co-production preparation method, is characterized in that: take Flower of Hollyhock as raw material, adopt extract, separation means, utilize and prepare step by step two kinds of tobacco aromatics using products with a collection of raw material, concrete technology step is as follows:
A. by dry Flower of Hollyhock, removal of impurities, pulverizing;
B. with certain density extraction using alcohol, the concentrated Flower of Hollyhock alcohol extract that to obtain;
C. the material slag after alcohol extracting adds a certain amount of ammonia soln heating to extract;
D. being cooled to after room temperature, is 3.5～5.0 with salt acid for adjusting pH value, adds a certain amount of zymin isothermal reaction for some time; Reheat lixiviate, after vat liquor concentrating under reduced pressure, obtain Flower of Hollyhock water extracting liquid.
2. Flower of Hollyhock extract co-production preparation method according to claim 1, is characterized in that: in step b, during extraction using alcohol, alcohol concn is 60 %～90 %, feed liquid mass ratio is 1:5～1:15, is heated to 60～85 ℃ and extracts 1～2 time, each 1～3 hour; Extracting solution is 10～50 % through being evaporated to paste containing amount.
3. Flower of Hollyhock extract co-production preparation method according to claim 1, it is characterized in that: in step c, ammonia concn used is 0.5 %～1.0 %, and add-on is 6～10 times of Flower of Hollyhock dry powder quality, and under 80～100 ℃ of conditions, heating is extracted 2～3 hours.
4. Flower of Hollyhock extract co-production preparation method according to claim 1, it is characterized in that: in steps d, the zymin adding is cellulase and polygalacturonase, addition is respectively 0.1～0.5 % and 0.5～1.0 % of Flower of Hollyhock dry powder quality, temperature constant temperature within the scope of 40～55 ℃ is set, enzymolysis time 1～3 hour; Enzyme digestion reaction post-heating to 80～100 ℃ further lixiviate 2～4 hours; Solid-liquid separation afterwards, gained clear liquid is 10～30 % through being evaporated to paste containing amount.
5. one kind is utilized Flower of Hollyhock extract prepared by the claim 1 method application in cigarette, it is characterized in that: Flower of Hollyhock alcohol extract is added in cigarette after ethanol and/or propylene glycol dilution, can increase Hui Tian, enrich note, reduce assorted gas, reduce the pungency of cigarette, concrete usage ratio is tobacco quality 0.01 ‰～0.1 ‰.
6. one kind is utilized Flower of Hollyhock extract prepared by the claim 1 method application in cigarette, it is characterized in that: Flower of Hollyhock water extracting liquid is applied on cigarette shreds with feed liquid after water dilution, while burning and sucking cigarette, flue gas free from extraneous odour, can enrichment flue gas, improve fragrance matter, increase sweet sense, reduce dry sensation, improve oral cavity comfortableness, concrete consumption is tobacco quality 0.01 ‰～0.5 ‰.
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| CN104862075A (en) * | 2015-06-03 | 2015-08-26 | 湖北中烟工业有限责任公司 | Preparation method of mullein extract for cigarette |
| CN105146715A (en) * | 2015-09-02 | 2015-12-16 | 云南中烟工业有限责任公司 | Method for improving cigarette moisturizing and aroma-improving effects by utilizing althaea rosea |
| CN108771282A (en) * | 2018-05-28 | 2018-11-09 | 河南中烟工业有限责任公司 | Application of the paulownia flower concrete in cigarette |
| CN111418883A (en) * | 2020-05-08 | 2020-07-17 | 河北瑞龙生物科技有限公司 | Tobacco flavor and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862075A (en) * | 2015-06-03 | 2015-08-26 | 湖北中烟工业有限责任公司 | Preparation method of mullein extract for cigarette |
| CN105146715A (en) * | 2015-09-02 | 2015-12-16 | 云南中烟工业有限责任公司 | Method for improving cigarette moisturizing and aroma-improving effects by utilizing althaea rosea |
| CN108771282A (en) * | 2018-05-28 | 2018-11-09 | 河南中烟工业有限责任公司 | Application of the paulownia flower concrete in cigarette |
| CN108771282B (en) * | 2018-05-28 | 2021-04-16 | 河南中烟工业有限责任公司 | Application of paulownia flower extract in cigarette |
| CN111418883A (en) * | 2020-05-08 | 2020-07-17 | 河北瑞龙生物科技有限公司 | Tobacco flavor and preparation method thereof |
| CN111418883B (en) * | 2020-05-08 | 2021-06-01 | 河北瑞龙生物科技有限公司 | Tobacco flavor and preparation method thereof |
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