CN109793262A - A kind of preparation method and applications of cigarette blackberry extract - Google Patents
A kind of preparation method and applications of cigarette blackberry extract Download PDFInfo
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- CN109793262A CN109793262A CN201910091403.4A CN201910091403A CN109793262A CN 109793262 A CN109793262 A CN 109793262A CN 201910091403 A CN201910091403 A CN 201910091403A CN 109793262 A CN109793262 A CN 109793262A
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- cigarette
- blackberry
- extract
- blackberry extract
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 66
- 239000000284 extract Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 244000078534 Vaccinium myrtillus Species 0.000 claims abstract description 85
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000047 product Substances 0.000 claims abstract description 32
- 235000003095 Vaccinium corymbosum Nutrition 0.000 claims abstract description 24
- 235000017537 Vaccinium myrtillus Nutrition 0.000 claims abstract description 24
- 235000021014 blueberries Nutrition 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 238000005360 mashing Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 241000208125 Nicotiana Species 0.000 claims description 22
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000012074 organic phase Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000005096 rolling process Methods 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 235000019505 tobacco product Nutrition 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 8
- 239000000654 additive Substances 0.000 abstract description 7
- 230000000996 additive effect Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 5
- 239000003546 flue gas Substances 0.000 abstract description 5
- 239000003205 fragrance Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 240000004307 Citrus medica Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 239000011285 coke tar Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The present invention provides a kind of preparation method and applications of cigarette blackberry extract, blackberry, blueberry is used to extract raw material, and blackberry, blueberry filters after crushing mashing, after filtrate n-hexane extraction, sloughs solvent;Filter residue is placed in alkaline aqueous solution and hydrolyzes, and is extracted after aqueous portion is dry with ethanol solution;The two is mixed in a certain ratio, and obtains cigarette blackberry extract.The present invention by a series of experimental studies of smokeing panel test shows the blackberry extract of addition, and in tobacco product suction, fragrance is abundant, flue gas is full, improves tobacco product mouthfeel.Invention increases blackberry, blueberry new effects and effect.For blackberry extract as additive of tobacco product, effect is obvious, there is " Chinese-style cigarette " product of distinctive style to have good application prospect exploitation.
Description
Technical field
The application that the present invention relates to natural plant extracts in tobacco product, specifically a kind of cigarette blackberry extract
Preparation method and applications.
Background technique
" Chinese-style cigarette " core competitiveness is to form selling point style, embodies personalized and differentiation, and it is wide to adapt to China
Big consumer's sucks habit and consumer need.Chinese style essence spice for cigarette is Chinese-style cigarette product " soul ", is Chinese style volume
Where the secret that cigarette style characteristic is formed.The scientifically flavoring and casing in cigarette, the personalized style of exactly prominent cigarette product
Important means.Meanwhile in order to improve the safety of smoking, lowering harm and decreasing coking has become an important composition portion of " Chinese-style cigarette "
Point.While reducing coke tar in cigarette, promotes and improve flue gas concentration and fragrance, also only by means of flavoring and casing technology.With
Chinese-style cigarette lowering harm and decreasing coking work go deep into, tobacco flavoring charging show its importance further.
The Chinese style essence spice for cigarette and new technology for constructing independent intellectual property right, extract flavors and fragrances from natural plants,
It allows the theory of health with the refined perfume (or spice) of cigarette, moves towards consumer together, be one of the basic research for developing " Chinese-style cigarette ".
For blackberry, blueberry rich in a variety of latent Studies of The Aromatic Substances such as flavonoids, cigarette perfume can be enriched by making an addition in cigarette product, make flue gas more
It is full.The present inventor has found in the course of the research: existing blackberry, blueberry extraction process is lower to the extraction efficiency of latent Studies of The Aromatic Substances and black
For the certain kind of berries in integrally extracting, being mixed into for the substances such as pectin can bring certain negative effect to cigarette product, increase separating technology again
The latent Studies of The Aromatic Substances of extraction can be damaged, to limit its purposes as cigarette additive.
Summary of the invention
The purpose of the present invention is to the deficiencies in the prior art, provide a kind of cigarette blackberry extract preparation method and
It is applied, and uses blackberry, blueberry to extract raw material, and blackberry, blueberry filters after crushing mashing, after filtrate n-hexane extraction, sloughs solvent;Filter
Slag is placed in alkaline aqueous solution and hydrolyzes, and is extracted after aqueous portion is dry with ethanol solution;The two is mixed in a certain ratio, and obtains cigarette
Use blackberry extract.
A kind of preparation method of cigarette blackberry extract, the specific steps are as follows:
(1) blackberry, blueberry cleaned up is placed in refiner, squeezes filtering after crushing mashing, obtains filtrate and filter residue;
(2) using n-hexane as extractant, the resulting filtrate of step (1) and n-hexane are filled according to mass ratio for 1:1~10
After dividing mixing, vibrate 1~5 hour, settle and separate goes out organic phase, and the organic phase after separation is concentrated into medicinal extract shape, sloughs completely just
Hexane is to get product 1;
(3) first alkali is added to the water, adjusting pH value is 8.0~12.0, and the weight ratio according still further to aqueous slkali and filter residue is
10~20:1 is mixed, and is heated 1~5 hour at 50~90 DEG C, and being eventually adding organic acid for adjusting pH value is 7.0, separation discharging
After liquid, feed liquid is concentrated into medicinal extract shape;
(4) using 70~95% ethyl alcohol as extractant, by the resulting medicinal extract of step (3) and ethyl alcohol according to mass ratio be 1:1~
10, it after being sufficiently mixed, vibrates 1~5 hour, filters to get product 2.
(5) product 1,2 is mixed in a certain ratio to get cigarette blackberry extract of the invention;In parts by mass, wherein
Product 1 is 10~40 parts, product 2 is 30~80 parts.
Further, the time of repose in the step (2) is 2 hours.
Further, the organic acid is acetic acid, citric acid, malic acid or citric acid.
Further, the alkali is sodium hydroxide, calcium hydroxide, potassium hydroxide or sodium carbonate.
Cigarette blackberry extract is added according to mass ratio 0.01%~0.05% for a kind of application of cigarette blackberry extract
Into the pipe tobacco of cigarette.
Further, cigarette blackberry extract is added in the pipe tobacco of cigarette according to mass ratio 0.02%~0.04%.
Further, cigarette is added to the specific steps of pipe tobacco with blackberry extract are as follows: be dissolved in blackberry extract cigarette molten
In agent, it will be sprayed on pipe tobacco, then evaporate molten during the pipe tobacco of production of cigarettes rolls dissolved with the solvent of blackberry extract
Agent.
Further, the solvent is the ethyl alcohol that mass concentration is 95%.
The present inventor shows that the blackberry extract of addition is aspirated in tobacco product by a series of experimental studies of smokeing panel test
Shi Xiangqi is abundant, flue gas is full, improves tobacco product mouthfeel.
Invention increases blackberry, blueberry new effects and effect.For blackberry extract as additive of tobacco product, effect is obvious,
There is " Chinese-style cigarette " product of distinctive style to have good application prospect exploitation.
Specific embodiment
Below in conjunction with specific embodiment, the technical solution in the present invention is clearly and completely described.
Embodiment 1
It uses blackberry, blueberry for raw material, the blackberry, blueberry cleaned up is placed in refiner, squeeze filtering after crushing mashing.With just oneself
Alkane is extractant, and n-hexane and filtrate quality ratio are 1, after being sufficiently mixed, and vibrates 5 hours, stands 2 hours, isolate organic phase,
Organic phase after separation is concentrated into medicinal extract shape, sloughs n-hexane completely to get product 1.
Filter residue hydrolysis, first adds sodium carbonate in water, and adjusting pH value is 8.0, and the weight ratio of water and filter residue is 20,50
DEG C heating 5 hours, be added second acid for adjusting pH value be 7.0, separate out-feed liquid after, feed liquid is concentrated into medicinal extract shape.With 70% ethyl alcohol
For extractant, ethyl alcohol and medicinal extract mass ratio are 1, after being sufficiently mixed, and vibrate 5 hours, filter to get product 2.
In parts by mass, wherein product 1 is 10 parts, product 2 is 30 parts, and mixing is extracted to get cigarette of the invention with blackberry, blueberry
Object.The extract can be used for additive of tobacco product.
Embodiment 2
It uses blackberry, blueberry for raw material, the blackberry, blueberry cleaned up is placed in refiner, squeeze filtering after crushing mashing.With just oneself
Alkane is extractant, and n-hexane and filtrate quality ratio are 10, after being sufficiently mixed, and vibrates 1 hour, stands 2 hours, isolate organic
Phase, the organic phase after separation are concentrated into medicinal extract shape, slough n-hexane completely to get product 1.
Sodium hydroxide, is first added to the water by filter residue hydrolysis, and adjusting pH value is 12.0, and the weight ratio of water and filter residue is 10,
It is heated 1 hour at 90 DEG C, it is 7.0 that lemon acid for adjusting pH value, which is added, and after separating out-feed liquid, feed liquid is concentrated into medicinal extract shape.With
95% ethyl alcohol is extractant, and ethyl alcohol and medicinal extract mass ratio are 10, after being sufficiently mixed, and vibrates 1 hour, filters to get product 2.
In parts by mass, wherein product 1 is 40 parts, product 2 is 40 parts, and mixing is extracted to get cigarette of the invention with blackberry, blueberry
Object.The extract can be used for additive of tobacco product.
Embodiment 3
It uses blackberry, blueberry for raw material, the blackberry, blueberry cleaned up is placed in refiner, squeeze filtering after crushing mashing.With just oneself
Alkane is extractant, and n-hexane and filtrate quality ratio are 5, after being sufficiently mixed, and vibrates 3 hours, stands 2 hours, isolate organic phase,
Organic phase after separation is concentrated into medicinal extract shape, sloughs n-hexane completely to get product 1.
Calcium hydroxide, is first added to the water by filter residue hydrolysis, and adjusting pH value is 9.0, and the weight ratio of water and filter residue is 12,
65 DEG C are heated 4 hours, and it is 7.0 that apple acid for adjusting pH value, which is added, and after separating out-feed liquid, feed liquid is concentrated into medicinal extract shape.With 75%
Ethyl alcohol is extractant, and ethyl alcohol and medicinal extract mass ratio are 3, after being sufficiently mixed, and vibrates 3 hours, filters to get product 2.
In parts by mass, wherein product 1 is 40 parts, product 2 is 80 parts, and mixing is extracted to get cigarette of the invention with blackberry, blueberry
Object.The extract can be used for additive of tobacco product.
Embodiment 4
It uses blackberry, blueberry for raw material, the blackberry, blueberry cleaned up is placed in refiner, squeeze filtering after crushing mashing.With just oneself
Alkane is extractant, and n-hexane and filtrate quality ratio are 8, after being sufficiently mixed, and vibrates 2 hours, stands 2 hours, isolate organic phase,
Organic phase after separation is concentrated into medicinal extract shape, sloughs n-hexane completely to get product 1.
Potassium hydroxide, is first added to the water by filter residue hydrolysis, and adjusting pH value is 11.0, and the weight ratio of water and filter residue is 17,
It is heated 1.5 hours at 75 DEG C, it is 7.0 that citron acid for adjusting pH value, which is added, and after separating out-feed liquid, feed liquid is concentrated into medicinal extract shape.With
85% ethyl alcohol is extractant, and ethyl alcohol and medicinal extract mass ratio are 8, after being sufficiently mixed, and vibrates 2 hours, filters to get product 2.
In parts by mass, wherein product 1 is 25 parts, product 2 is 60 parts, and mixing is extracted to get cigarette of the invention with blackberry, blueberry
Object.The extract can be used for additive of tobacco product.Using the cigarette blackberry, blueberry that above method preparation is added in the pipe tobacco to cigarette
Extract
Pipe tobacco is added with blackberry extract in cigarette during the pipe tobacco of production of cigarettes rolls.The blackberry, blueberry being added into pipe tobacco
Extract accounts for the 0.03% of pipe tobacco weight.Specific method is first blackberry extract to be dissolved in the ethyl alcohol that mass concentration is 95%,
Diluted Alcohol dissolved with blackberry extract is uniformly sprayed on pipe tobacco, subsequent ethanol evaporation is fallen.Pipe tobacco rolls into inspection through cigarette machine
Sample cigarette.
Effect experiment in cigarette smoke
40 grams two parts of finished cut tobacco balanced at 22 DEG C ± 1 DEG C of temperature and relative humidity (RH) 60% ± 2% are taken, are pressed
The 0.04% of its quality weighs cigarette blackberry extract, after the dilution of 95% ethyl alcohol, is equably sprayed on pipe tobacco with larynx jet pipe,
Flavoring and non-aromatic tobacco sample are placed in the climatic chamber of 22 DEG C ± 1 DEG C of temperature and RH60% ± 2% and balance 48 hours, use
It fills out cigarette device and cigarette is made in the pipe tobacco of flavoring and non-flavoring respectively, then balance 48 is small under 22 DEG C ± 1 DEG C and RH60% ± 2%
When, ask cigarette sensory evaluating smoking group to be smoked panel test.
The personnel that smoke panel test unanimously think the blackberry extract being added, and in tobacco product suction, fragrance is abundant, flue gas is full, changes
Kind tobacco product mouthfeel.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Belong to those skilled in the art in the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, all answers
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be subject to the protection scope in claims.
Claims (8)
1. a kind of preparation method of cigarette blackberry extract, it is characterised in that specific step is as follows:
(1) blackberry, blueberry cleaned up is placed in refiner, squeezes filtering after crushing mashing, obtains filtrate and filter residue;
(2) using n-hexane as extractant, being that 1:1~10 are abundant according to mass ratio by the resulting filtrate of step (1) and n-hexane is mixed
After conjunction, vibrating 1~5 hour, settle and separate goes out organic phase, and the organic phase after separation is concentrated into medicinal extract shape, n-hexane is sloughed completely,
Up to product 1;
(3) first alkali is added to the water, adjust pH value be 8.0~12.0, according still further to the weight ratio of aqueous slkali and filter residue be 10~
20:1 is mixed, and is heated 1~5 hour at 50~90 DEG C, and being eventually adding organic acid for adjusting pH value is 7.0, after separating out-feed liquid,
Feed liquid is concentrated into medicinal extract shape;
(4) using 70~95% ethyl alcohol as extractant, according to mass ratio it is 1:1~10 by the resulting medicinal extract of step (3) and ethyl alcohol, fills
It after dividing mixing, vibrates 1~5 hour, filters to get product 2.
(5) product 1,2 is mixed in a certain ratio to get cigarette blackberry extract of the invention;In parts by mass, wherein product
1 is 10~40 parts, product 2 is 30~80 parts.
2. a kind of preparation method of cigarette blackberry extract according to claim 1, it is characterised in that: the step (2)
In time of repose be 2 hours.
3. a kind of preparation method of cigarette blackberry extract according to claim 1, it is characterised in that: the organic acid is
Acetic acid, citric acid, malic acid or citric acid.
4. a kind of preparation method of cigarette blackberry extract according to claim 1, it is characterised in that: the alkali is hydrogen-oxygen
Change sodium, calcium hydroxide, potassium hydroxide or sodium carbonate.
5. a kind of application of the cigarette blackberry extract prepared such as any one of claim 1-4 the method, it is characterised in that: will
Cigarette blackberry extract is added in the pipe tobacco of cigarette according to mass ratio 0.01%~0.05%.
6. a kind of application of cigarette blackberry extract as claimed in claim 5, it is characterised in that: press cigarette with blackberry extract
It is added in the pipe tobacco of cigarette according to mass ratio 0.02%~0.04%.
7. a kind of application of cigarette blackberry extract as claimed in claim 5, it is characterised in that: add cigarette blackberry extract
Enter the specific steps of pipe tobacco are as follows: cigarette is dissolved in solvent with blackberry extract, it will be raw in cigarette dissolved with the solvent of blackberry extract
The pipe tobacco of production is sprayed on pipe tobacco during rolling, and then evaporates solvent.
8. a kind of application of cigarette blackberry extract as claimed in claim 7, it is characterised in that: the solvent is mass concentration
For 95% ethyl alcohol.
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CN201910091403.4A CN109793262B (en) | 2019-01-30 | 2019-01-30 | Preparation method and application of blackberry extract for cigarettes |
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