CN102090712B - Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes - Google Patents
Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes Download PDFInfo
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- CN102090712B CN102090712B CN 201010619928 CN201010619928A CN102090712B CN 102090712 B CN102090712 B CN 102090712B CN 201010619928 CN201010619928 CN 201010619928 CN 201010619928 A CN201010619928 A CN 201010619928A CN 102090712 B CN102090712 B CN 102090712B
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Abstract
The invention relates to a method for preparing a coarse extract of peanut shell total flavones. The method comprises the following steps of: crushing cleaned peanut shells, degreasing the peanut shells with ethyl acetate, centrifuging, adding distilled water into the residue for water bath stirring extraction, centrifuging extraction solution and concentrating to obtain concentrated solution, performing alcohol sedimentation and centrifuging to obtain the coarse extract of peanut shell total flavones, concentrating the coarse extract, adding propylene glycol into the coarse extract for mixing, and applying the mixture and extracted residue which serve as an additive for cigarettes to cigarettes according to certain percentage.
Description
[technical field]
The present invention relates to compound and extract the field.More specifically, the present invention relates to a kind of preparation method of coarse extract of peanut shell total flavones, also relate to the application of described general flavone crude extract in cigarette.
[background technology]
Tobacco business is when utilizing the raw materials such as discarded tobacco leaf, reconstituted tobacoo and expanded cut stem to produce product, and its product quality is still relatively poor.Along with the reduction of cigarette tar content, the fragrance of cigarette descends, and mouth or throat's dry sensation strengthen, and have restricted the lifting of domestic cigarette product quality.After reducing the T/N amount, how keeping the cigarette product style and features, embody high fragrance and the satisfaction of Chinese-style cigarette, is to face key problems-solving in the low-coke tar cigarette development process.
China is Peanut big producing country, year secondary nearly 4,000,000 tons of the peanut shell of producing, account for peanut heavy about 30%.These peanut shells are except a minority partly is used as feed and fuel, and major part is all thrown away in vain, and this has caused the significant wastage of resource.
Peanut shell is the shell of dicotyledonous fruits of leguminous plants, is a kind of Chinese herbal medicine, includes in Compendium of Material Medica, has the effect of astringeing the lung to stop cough, and is used for chronic cough asthma on the traditional Chinese medical science, coughs sputum streaked with blood.Itself does not have fragrance peanut shell, but has obvious nutty after the baking.Studies show that, except containing a large amount of carbohydrate and fiber, also contain flavone compound in the peanut shell, this flavonoids effective constituent has anti-inflammatory, cough-relieving dispel nitrogen, the effect such as anti-oxidant.The Flavonoid substances that extracts from peanut shell can be used as edible antioxidant and flavor enhancement.With the flavonoids polyphenoils in the buck method extraction peanut shell, the relative recovery rate 72.76% of general flavone.Not only Product Activity is high, form good (Powdered), recovery rate is high, and reparation technology is simple, and production cost is much lower than organic solvent, heat endurance that the more important thing is product is fabulous, even deposit 120min under 185 ℃, its antioxidation activity only descends 19%, deposits 40min, its antioxidation activity only descends 5.8%, and this advantage has practical significance for food processing.
2005, the people such as the fragrant Jakob P.Ley of International Flavors ﹠ Fragrances Inc.'s moral passed through research and find, Luteolin from Peanut (5,7,3 ', 4 '-kaempferol) have antibechic and phlegm-dispelling functions, being applied in the food is a kind of good bitter taste masking agent.In recent years, the application in cigarette conducts a research the technical staff of Hua Bao group to flavone compound in the herbal mixture, extracts the natural flavone compounds in the composite Chinese medicinal formulae, is prepared into cigarette additive through allotment.Final evaluation experimental shows, Chinese medicine compound prescription through cigarette pyroreaction (Maillard reaction) afterwards, the active ingredient of release more can significantly alleviate throat and stimulate, and coordinates fragrance, increases the oral cavity comfort level.
In cigarette, has the fact of covering bitter taste, promoting the production of body fluid, moisturize effect based on the natural flavone compounds, the applicant attempts extracting by the peanut shell flavone class material to cheapness first, and extract is directly used in cigarette (tobacco leaf, stem, thin slice), in the hope of reaching the purpose that promotes tobacco leaf, stem, thin slice quality.
[summary of the invention]
[problem that invention will solve]
The preparation method who the purpose of this invention is to provide a kind of coarse extract of peanut shell total flavones.
Another object of the present invention is a kind of coarse extract of peanut shell total flavones.
Another object of the present invention provides the application of described coarse extract of peanut shell total flavones in cigarette.
[technical scheme]
The present invention relates to a kind of preparation method of coarse extract of peanut shell total flavones, it is characterized in that it may further comprise the steps:
(1) clean peanut shell is pulverized, and powder is crossed behind the 20-100 mesh sieve and infiltrated with ethyl acetate, and mechanical agitation 1 hour at room temperature, then leaves standstill 0.5 hour;
(2) mixture that obtains of step (1) filters, and removes the ethyl acetate suspension, obtains the peanut shell residue, adds distilled water in the residue, heating water bath, mechanical agitation 2-5 hour;
(3) extract that obtains of step (2) cools off, and filters and removes residue, and is then centrifugal, obtains clarified solution;
(4) clarified solution that obtains of step (3) adds ethanol when being evaporated to former extract 1/7-1/8 volume, and placement is spent the night;
(5) precipitation solution that obtains of step (4) is carried out centrifugally, obtains alcohol precipitation clear liquid and sediment, allocates with propane diols after the alcohol precipitation clear liquid is concentrated, obtains major product I, and obtaining residue after water extraction is filtered is byproduct II.
A preferred embodiment of the invention, in the step (1), the amount of ethyl acetate is weighing scale 3-5 times with the peanut shell powder.
According to another kind of preferred embodiment of the present invention, in the step (2), the amount of the distilled water of adding is weighing scale 8-10 times with residue.
According to another kind of preferred embodiment of the present invention, in the step (2), the bath temperature during mechanical agitation is 80-90 ℃.
According to another kind of preferred embodiment of the present invention, in the step (3), centrifugal speed is 3000r/min, centrifugal 30 minutes.
According to another kind of preferred embodiment of the present invention, the ethanol that adds in the step (4) is 90% ethanol, addition and initial feed equivalent.
According to another kind of preferred embodiment of the present invention, the addition of propane diols is the 5%-10% of material quantity in the step (5).
The invention still further relates to a kind of coarse extract of peanut shell total flavones major product I and byproduct residual II for preparing according to the above method.
The invention still further relates to the application of described coarse extract of peanut shell total flavones in cigarette, wherein major product I and byproduct residual II are added to respectively in tobacco leaf, stem and the thin slice.
According to another kind of preferred embodiment of the present invention, major product I and the adding proportion of byproduct residual II in cigarette are weight ratio 1: 10-15, add up to the 0.1-0.3% that is added to according to cigarette weight.
[beneficial effect]
The inventive method has following beneficial effect:
1, coarse extract of peanut shell total flavones is added in the tobacco leaf, in the cigarette perfume (or spice) that keeps tobacco leaf itself, has improved the fresh and sweet alcohol sense of flue gas, also so that flue gas becomes softer, graceful, reduced bitter taste.
Application on the cigarette can be sprayed at tobacco leaf, stem or is coated on the reconstituted tobacoo according to conventional perfuming process program, then in climatic chamber balance 24-48 hour, plays cigarette or chopping again and beats cigarette and make cigarette.Smoking result sees Table 1-3.
The sensory evaluation of table 1 tobacco sample
The sensory evaluation of table 2 stem sample
The sensory evaluation of table 3 thin slice sample
2, preparation method of the present invention is easy, and production equipment requires low, draws materials extensively, is applicable to large-scale industrial production.
[specific embodiment]
Following non-limiting example is used for illustrating in greater detail the present invention.
Embodiment 1
(1) peanut shell of choosing after cleaning up is pulverized after drying, excessively behind 40 mesh sieves, gets 100g peanut shell powder, in powder weight, be that 370g ethyl acetate infiltrates degreasing with 3.7 times, mechanical agitation 1 hour at room temperature then, left standstill again 0.5 hour, and obtained the 470g mixture;
(2) the 470g mixture that obtains of step (1) filters, and removes the ethyl acetate suspension, obtains the peanut shell residue, adds 1000mL distilled water in the residue, heating water bath to 85 ℃, and mechanical agitation 3.5 hours obtains the 800mL extract;
(3) the 800mL extract that obtains of step (2) cools off, and filters and removes residue, then with the centrifugal 30min of 3000r/min speed, obtains the 780mL clarified solution;
(4) the 780mL clarified solution that obtains of step (3) adds 90% ethanol of 200mL when being evaporated to former extract 1/7 volume, and placement is spent the night;
(5) precipitation solution that obtains of step (4) is carried out centrifugal, obtain alcohol precipitation clear liquid 360mL and sediment 4.0g, the alcohol precipitation clear liquid is after suitably concentrating, with 10mL 99.9%1, the 2-propane diols is allocated, obtain 50mL major product I, obtain residue after water extraction is filtered and be byproduct II 120g (weight in wet base).
Embodiment 2
(1) peanut shell of choosing after cleaning up is pulverized after drying, excessively behind 80 mesh sieves, gets 100g peanut shell powder, in powder weight, be that 500g ethyl acetate infiltrates degreasing with 5 times, mechanical agitation 1 hour at room temperature then, left standstill again 0.5 hour, and obtained the 600g mixture;
(2) the 600g mixture that obtains of step (1) filters, and removes the ethyl acetate suspension, obtains the peanut shell residue, adds 800mL distilled water in the residue, heating water bath to 90 ℃, and mechanical agitation 4.5 hours obtains the 810mL extract;
(3) the 810mL extract that obtains of step (2) cools off, and filters and removes residue, then with the centrifugal 30min of 3000r/min speed, obtains the 790mL clarified solution;
(4) the 790mL clarified solution that obtains of step (3) adds 200mL90% ethanol when being evaporated to former extract 1/8 volume, and placement is spent the night;
(5) precipitation solution that obtains of step (4) is carried out centrifugal, obtain alcohol precipitation clear liquid 298mL and sediment 4.5g, the alcohol precipitation clear liquid is used 10mL99.9%1 after suitably concentrating, the 2-propane diols is allocated, obtain major product I 45mL, obtain residue after water extraction is filtered and be byproduct II 125g (weight in wet base).
Claims (10)
1. the preparation method of a coarse extract of peanut shell total flavones is characterized in that it may further comprise the steps:
(1) clean peanut shell is pulverized, and powder is crossed behind the 20-100 mesh sieve and infiltrated with ethyl acetate, and mechanical agitation 1 hour at room temperature, then leaves standstill 0.5 hour;
(2) mixture that obtains of step (1) filters, and removes the ethyl acetate suspension, obtains the peanut shell residue, adds distilled water in the residue, and heating water bath mechanical agitation 2-5 hour, obtains extract;
(3) extract that obtains of step (2) cools off, and filters and removes residue, and is then centrifugal, obtains clarified solution;
(4) clarified solution that obtains of step (3) adds ethanol when being evaporated to former extract 1/7-1/8 volume, and placement is spent the night;
(5) precipitation solution that obtains of step (4) is carried out centrifugally, obtains alcohol precipitation clear liquid and sediment, and the alcohol precipitation clear liquid is allocated with propane diols after concentrated, obtains major product I, and filtering the residue of removing in the described step (3) is byproduct II.
2. method according to claim 1 is characterized in that in the step (1), and the amount of ethyl acetate is weighing scale 3-5 times with the peanut shell powder.
3. method according to claim 1 is characterized in that in the step (2), and the amount of the distilled water of adding is weighing scale 8-10 times with the peanut shell residue in the step (2).
4. method according to claim 1 is characterized in that in the step (2), the bath temperature during mechanical agitation is 80-90 ℃.
5. method according to claim 1 is characterized in that centrifugal speed is 3000r/min in the step (3), centrifugal 30 minutes.
6. a method according to claim 1 is characterized in that the ethanol that adds in the step (4) is 90% ethanol, and addition is the peanut shell powder 200ml of every 100g through pulverizing.
7. a method according to claim 1 is characterized in that the concentration of propane diols in the step (5) is 99.9%, and addition is the peanut shell powder 10ml of every 100g through pulverizing.
One kind according to claim 1-7 in the described method of each claim the coarse extract of peanut shell total flavones major product I and the byproduct residual II that prepare.
9. the application of coarse extract of peanut shell total flavones according to claim 8 in cigarette is characterized in that major product I and byproduct residual II add to respectively in tobacco leaf, stem and the thin slice.
10. application according to claim 9, it is characterized in that major product I and the adding proportion of byproduct residual II in cigarette are weight ratio 1:10-15, add up to the 0.1-0.3% that is added to according to cigarette weight, be cigarette additive, be applied in the cigarette with certain proportion.
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| CN 201010619928 CN102090712B (en) | 2010-12-29 | 2010-12-29 | Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes |
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| CN 201010619928 CN102090712B (en) | 2010-12-29 | 2010-12-29 | Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes |
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| CN102090712B true CN102090712B (en) | 2013-01-23 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102613692B (en) * | 2012-04-16 | 2014-09-10 | 华宝食用香精香料（上海）有限公司 | Method for recycling tobacco flavor from cigarette production waste |
| CN102823939B (en) * | 2012-09-17 | 2016-03-30 | 福建中烟工业有限责任公司 | A kind of preparation method of wild eggplant leaf extract and the application in cigarette thereof |
| US11412775B2 (en) | 2012-10-09 | 2022-08-16 | R.J. Reynolds Tobacco Company | Tobacco-derived composition |
| 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 |
| CN104585871B (en) * | 2015-01-20 | 2016-02-03 | 川渝中烟工业有限责任公司 | The anti-oxidant tobacco juice for electronic smoke of a kind of Hippophate flavone |
| 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 |
| CN110477445A (en) * | 2019-08-28 | 2019-11-22 | 广东香龙香料有限公司 | Flavouring essence for tobacco containing wolfberry fruit extract |
| CN112439001A (en) * | 2020-12-22 | 2021-03-05 | 长江绿银(无锡)科技有限公司 | Method for extracting flavonoid compounds from alternanthera philoxeroides |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1225998C (en) * | 2003-08-19 | 2005-11-09 | 广东神农烟科技术有限公司 | Cigarette additive extracted from natural plant, and extracting method and use in cigarette thereof |
| CN101514302B (en) * | 2008-02-20 | 2012-02-29 | 湖北中烟工业有限责任公司 | Method for comprehensively utilizing peanut shell |
| CN101579146B (en) * | 2008-05-12 | 2012-07-04 | 湖北中烟工业有限责任公司 | Method for preparing tobacco flavor by Maillard reaction of nitrogen source and sugar source |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee before: Huabao flavor Ltd. |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: Huabao flavor Ltd. Address before: 201821 Yecheng Road, Shanghai, No. 1299, No. Patentee before: Huabao Flavours & Fragrances Co.,Ltd |
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Effective date of registration: 20170112 Address after: 335000 Yingtan economic and Technological Development Zone, Longgang District, South Wing Road, Jiangxi Patentee after: YINGTAN HUABAO ESSENCE CO.,LTD. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee before: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. |