CN108102787A - A kind of Damask Rose tobacco aromaticss and its preparation method and application - Google Patents

A kind of Damask Rose tobacco aromaticss and its preparation method and application Download PDF

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Publication number
CN108102787A
CN108102787A CN201810038174.5A CN201810038174A CN108102787A CN 108102787 A CN108102787 A CN 108102787A CN 201810038174 A CN201810038174 A CN 201810038174A CN 108102787 A CN108102787 A CN 108102787A
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Prior art keywords
damask rose
extracting solution
tobacco aromaticss
rose
damask
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CN201810038174.5A
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郑屹
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YUNNAN SHENBOYUAN BIOLOGICAL TECHNOLOGY Co Ltd
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YUNNAN SHENBOYUAN BIOLOGICAL TECHNOLOGY Co Ltd
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Priority to CN201810038174.5A priority Critical patent/CN108102787A/en
Publication of CN108102787A publication Critical patent/CN108102787A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303Plant extracts other than tobacco
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Agronomy & Crop Science (AREA)
  • Botany (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

A kind of Damask Rose tobacco aromaticss and its preparation method and application, it is characterized in that, the fragrance is using Damask Rose as raw material, it adds in after mixed solvent and carries out extracting solution extraction, concentration, dilution, absorption, elution and enrichment process again, Damask Rose tobacco aromaticss are made, compared with traditional extracting method, use mixed solvent ultrasonic wave extraction Damask Rose, greatly reduce heating time, / 10th of only traditional steam distillation, recovery rate is also obviously improved, and significantly reduces the production cost of rose extract;It is separated with reference to the elution of macroporous absorbent resin, reducing has cigarette smoke in extract the content of negative effect ingredient, improve the quality and purity of active ingredient, think through smokeing panel test, the product can be promoted cigarette flavor matter, cigarette perfume alcohol and exquisiteness, flue gas moisture feeling and pleasant impression aspect also have clear improvement.

Description

A kind of Damask Rose tobacco aromaticss and its preparation method and application
Technical field
The present invention relates to cigarette additive technical field more particularly to a kind of Damask Rose tobacco aromaticss and its preparations Methods and applications.
Background technology
Damask Rose originates in Syria, starts in 14th century widely to plant in France, and Damask Rose is to protect to add The main rose variety and universally acknowledged high-quality rose variety of Leah plantation.Blade is celadon, is had on scape hard Hair;Hose-in-hose is opened, petal edge color is slightly shallow, there is the texture as silks and satins;Purely, the careful fragrance of a flower makes its hat pressure beautiful and fragrant flowers, becomes Top grade in rose for oil is widely cultivated to extract Rosa Damascana at present at home.
The chemical composition of Rosa Damascana is one of most complicated essential oil of ingredient, it is known that ingredient is more than more than 300 kinds.Rosa Damascana Main chemical composition includes citronellol, phenylethanol, geraniol, nerol, ethylalbenzene, farnesol(Fanesol), rose Rare wax, micro nonyl alcohol, linalool, aldehyde C-9, citral, carvol, acetic acid lemongrass, methyleugenol, eugenol.Its energy The immune and nervous system with landman is stimulated, while helps to improve the secretion of incretory, organ sclerosis is removed, repairs carefully Born of the same parents.
Rosa Damascana is the essential oil of most expensive in the world, and per kilogram price is up to more than 20,000 U.S. dollars.Traditional Rosa Damascana is adopted It is produced with steam distillation, expends substantial amounts of manpower and materials, and yield is extremely low, it is difficult to be widely used in perfuming cigarette technique In, only have a small amount of application in the essence of high-grade cigarette at present, the aroma quality of cigarette flavor can be promoted, make cigarette perfume alcohol and it is fine and smooth, It also has clear improvement in terms of flue gas moisture feeling and pleasant impression, therefore according to the characteristics of perfuming cigarette, exploitation low price, the extraction of applicable rose Object has a vast market prospect, is subject to the extensive concern of tobacco aromaticss insider.
The content of the invention
The technical problems to be solved by the invention are, for current traditional Rosa Damascana steam distillation use to produce with Tobacco aromaticss are made and there is the problem of of high cost, low output, a kind of Damask Rose tobacco aromaticss and its preparation side are provided Method and application.
A kind of Damask Rose tobacco aromaticss, which is characterized in that the fragrance is using Damask Rose as raw material, is added in Extracting solution extraction, concentration, dilution, absorption, elution and enrichment process again are carried out after mixed solvent, with obtained Damask Rose cigarette Use fragrance.
Preferably, the Damask Rose raw material is Damask Rose of the moisture in 8wt% -12wt%.
The present invention also provides a kind of preparation methods of Damask Rose tobacco aromaticss, it is characterised in that the preparation The step of method, is as follows:
(1)Damask Rose petal is added in ultrasonic extraction tank, it is molten to add in the mixing being made of ethyl alcohol, propylene glycol, water The feed liquid weight ratio of agent, Damask Rose petal and mixed solvent is 1:4—1:10, open ultrasonic extraction tank, ultrasonic wave Frequency is 50-200kHz, and temperature is maintained at 40-60 DEG C, and 30-60 minutes extraction times extracting solution is made, stopped operation, Extracting solution is poured out after slightly cooling down, is filtered with strainer, collection obtains first time extracting solution, collects remaining residue, remaining residue It repeats the above method and carries out second of extraction, be collected by filtration to obtain second of extracting solution;
(2)After mixing first time extracting solution and second of extracting solution, extracting solution is poured into rotary evaporator and is concentrated, concentrated Temperature is 45-55 DEG C, and vacuum degree is 0.005-0.01Mpa, concentrate is made;
(3)The obtained concentrate distilled water of 10-15 times of weight is diluted, dilution is made;
(4)Dilution is passed to DM301 types large pore resin absorption column to carry out absorption process with the flow velocity of 1.5BV/h, absorption After, resin column is rinsed with the flow velocity of 1.0BV/h with 10L distilled water, after flushing, with the flow velocity of 1.0-1.5BV/h, is used The ethanol water elution agent elution of 20wt%-60wt% of 1.5-2.0BV, collects eluent;
(5)By step(4)The eluent of middle collection, which is poured into rotary evaporator, to be concentrated, 45-55 DEG C of thickening temperature, vacuum 0.005-0.01Mpa is spent, is concentrated into density as 1.100-1.250 to get to Damask Rose tobacco aromaticss.
Preferably, the step(1)In mixed solvent contained by ethyl alcohol be 20-30 mass parts, propylene glycol is 10-20 matter Amount part, water are:40-60 mass parts.
Preferably, the step(4)In Dm301 types macroporous absorbent resin with after 95% ethyl alcohol soaked overnight, with distillation Water is rinsed to no ethanol flavor, then impregnates 4h with the solution of 4%NaOH, with distilled water flushing to neutrality;It is finally molten with 4% HCl Liquid impregnates 4h, and with distilled water flushing to neutrality, dress column is spare, and cylinder specification is 10cm × 60cm.
The present invention also provides a kind of applications of Damask Rose tobacco aromaticss, which is characterized in that wherein presses 0.03wt% -0.1wt% of cigarette shreds weighs Damask Rose tobacco aromaticss, after being dissolved with 30wt% ethanol waters, spray It is added in flue-cured tobacco pipe tobacco.
A kind of Damask Rose tobacco aromaticss of the present invention and its preparation method and application, with traditional extracting method phase Than using mixed solvent ultrasonic wave extraction Damask Rose, greatly reducing heating time, being only traditional steam distillation 1/10th, recovery rate is also obviously improved, and significantly reduces the production cost of rose extract;With reference to macroporous absorbent resin Elution separation, reduce the content for having negative effect ingredient in extract to cigarette smoke, improve the quality of active ingredient And purity, think through smokeing panel test, which can make the promotion of cigarette flavor matter, cigarette perfume alcohol and exquisiteness, flue gas moisture feeling and pleasant impression aspect Also have clear improvement.
Specific embodiment
With reference to specific embodiment, the present invention will be described in further detail.
Embodiment 1:
A kind of the step of Damask Rose tobacco aromaticss, the tobacco aromaticss preparation method, is as follows:
(1)1000g Damask Rose petals are added in ultrasonic extraction tank, addition weight ratio is ethyl alcohol:Propylene glycol:Water= 30:10:The feed liquid weight ratio of 60 mixed solvent, Damask Rose petal and mixed solvent is 1:10, it opens ultrasonic wave and carries Tank, ultrasonic frequency 50Hz are taken, temperature is maintained at 45 DEG C, and 50 minutes extraction times extracting solution is made, stopped operation, slightly Extracting solution is poured out after cooling, is filtered with strainer, collection obtains first time extracting solution, collects remaining residue, remaining residue weight The multiple above method carries out second and extracts, and is collected by filtration to obtain second of extracting solution;
(2)After mixing first time extracting solution and second of extracting solution, extracting solution is poured into rotary evaporator and is concentrated, concentrated Temperature is 55 DEG C, vacuum degree 0.005Mpa, concentrate is made;
(3)Obtained concentrate is diluted with 10 times of distilled water, dilution is made;
(4)Dilution is passed to DM301 types large pore resin absorption column to carry out absorption process with the flow velocity of 1.5BV/h, absorption After, resin column is rinsed with the flow velocity of 1.0BV/h with 10L distilled water, after flushing, with the flow velocity of 1.5BV/h, is used The ethanol water elution agent elution of the 20wt% of 1.5BV, collects eluent;
(5)By step(4)The eluent of middle collection, which is poured into rotary evaporator, to be concentrated, 50 DEG C of thickening temperature, vacuum degree 0.005Mpa is concentrated into density as 1.150 to get to Damask Rose tobacco aromaticss.
The Damask Rose tobacco aromaticss of gained by the 0.03wt% of cigarette shreds are weighed, are dissolved with 30% ethyl alcohol, It is uniformly sprayed onto in pipe tobacco, cigarette, which is made, to pipe tobacco smokes panel test, and smoking result is as shown in table 1:
Embodiment 2:
A kind of the step of Damask Rose tobacco aromaticss, the tobacco aromaticss preparation method, is as follows:
(1)1000g Damask Rose petals are added in ultrasonic extraction tank, addition weight ratio is ethyl alcohol:Propylene glycol:Water= 20:20:The feed liquid weight ratio of 60 mixed solvent, Damask Rose petal and mixed solvent is 1:6, open ultrasonic wave extraction Tank, ultrasonic frequency 100Hz, temperature are maintained at 50 DEG C, and 40 minutes extraction times extracting solution is made, stopped operation, slightly cold But extracting solution is poured out afterwards, is filtered with strainer, and collection obtains first time extracting solution, collects remaining residue, and remaining residue repeats The above method carries out second and extracts, and is collected by filtration to obtain second of extracting solution;
(2)After mixing first time extracting solution and second of extracting solution, extracting solution is poured into rotary evaporator and is concentrated, concentrated Temperature is 55 DEG C, vacuum degree 0.01Mpa, concentrate is made;
(3)Obtained concentrate is diluted with 15 times of distilled water, dilution is made;
(4)Dilution is passed to DM301 types large pore resin absorption column to carry out absorption process with the flow velocity of 1.5BV/h, absorption After, resin column is rinsed with the flow velocity of 1.0BV/h with 10L distilled water, after flushing, with the flow velocity of 1.0BV/h, is used The ethanol water elution agent elution of the 40wt% of 2.0BV, collects eluent;
(5)By step(4)The eluent of middle collection, which is poured into rotary evaporator, to be concentrated, 55 DEG C of thickening temperature, vacuum degree 0.01Mpa is concentrated into density as 1.20 to get to Damask Rose tobacco aromaticss.
The Damask Rose tobacco aromaticss of gained by the 0.03wt% of cigarette shreds are weighed, are dissolved with 30% ethyl alcohol, It is uniformly sprayed onto in pipe tobacco, cigarette, which is made, to pipe tobacco smokes panel test, and smoking result is as shown in table 2:
Embodiment 3:
A kind of the step of Damask Rose tobacco aromaticss, the tobacco aromaticss preparation method, is as follows:
(1)1000g Damask Rose petals are added in ultrasonic extraction tank, addition weight ratio is ethyl alcohol:Propylene glycol:Water= 30:20:The feed liquid weight ratio of 50 mixed solvents, Damask Rose petal and mixed solvent is 1:4, open ultrasonic wave extraction Tank, ultrasonic frequency 200Hz, temperature are maintained at 60 DEG C, and 60 minutes extraction times extracting solution is made, stopped operation, slightly cold But extracting solution is poured out afterwards, is filtered with strainer, and collection obtains first time extracting solution, collects remaining residue, and remaining residue repeats The above method carries out second and extracts, and is collected by filtration to obtain second of extracting solution;
(2)After mixing first time extracting solution and second of extracting solution, extracting solution is poured into rotary evaporator and is concentrated, concentrated Temperature is 55 DEG C, vacuum degree 0.005Mpa, concentrate is made;
(3)Obtained concentrate is diluted with 15 times of distilled water, dilution is made;
(4)Dilution is passed to DM301 types large pore resin absorption column to carry out absorption process with the flow velocity of 1.5BV/h, absorption After, resin column is rinsed with the flow velocity of 1.0BV/h with 10L distilled water, after flushing, with the flow velocity of 1.5BV/h, is used The ethanol water elution agent elution of the 60wt% of 2.0BV, collects eluent;
(5)By step(4)The eluent of middle collection, which is poured into rotary evaporator, to be concentrated, 55 DEG C of thickening temperature, vacuum degree 0.005Mpa is concentrated into density as 1.250 to get to Damask Rose tobacco aromaticss.
The Damask Rose tobacco aromaticss of gained by the 0.03wt% of cigarette shreds are weighed, are dissolved with 30% ethyl alcohol, It is uniformly sprayed onto in pipe tobacco, cigarette, which is made, to pipe tobacco smokes panel test, and smoking result is as shown in table 3:

Claims (6)

1. a kind of Damask Rose tobacco aromaticss, which is characterized in that the fragrance is using Damask Rose as raw material, is added in mixed Extracting solution extraction, concentration, dilution, absorption, elution and enrichment process again are carried out after bonding solvent, Damask Rose cigarette use is made Fragrance.
A kind of 2. Damask Rose tobacco aromaticss according to claim 1, it is characterised in that Damascus rose Rare raw material is Damask Rose of the moisture in 8wt% -12wt%.
3. a kind of preparation method of Damask Rose tobacco aromaticss, it is characterised in that the step of described preparation method is as follows:
(1)Damask Rose petal is added in ultrasonic extraction tank, it is molten to add in the mixing being made of ethyl alcohol, propylene glycol, water The feed liquid weight ratio of agent, Damask Rose petal and mixed solvent is 1:4—1:10, open ultrasonic extraction tank, ultrasonic wave Frequency is 50-200kHz, and temperature is maintained at 40-60 DEG C, and 30-60 minutes extraction times extracting solution is made, stopped operation, Extracting solution is poured out after slightly cooling down, is filtered with strainer, collection obtains first time extracting solution, collects remaining residue, remaining residue It repeats the above method and carries out second of extraction, be collected by filtration to obtain second of extracting solution;
(2)After mixing first time extracting solution and second of extracting solution, extracting solution is poured into rotary evaporator and is concentrated, concentrated Temperature is 45-55 DEG C, and vacuum degree is 0.005-0.01Mpa, concentrate is made;
(3)The obtained concentrate distilled water of 10-15 times of weight is diluted, dilution is made;
(4)Dilution is passed to DM301 types large pore resin absorption column to carry out absorption process with the flow velocity of 1.5BV/h, absorption After, resin column is rinsed with the flow velocity of 1.0BV/h with 10L distilled water, after flushing, with the flow velocity of 1.0-1.5BV/h, is used The ethanol water elution agent elution of 20wt%-60wt% of 1.5-2.0BV, collects eluent;
(5)By step(4)The eluent of middle collection, which is poured into rotary evaporator, to be concentrated, 45-55 DEG C of thickening temperature, vacuum 0.005-0.01Mpa is spent, is concentrated into density as 1.100-1.250 to get to Damask Rose tobacco aromaticss.
4. the preparation method of a kind of Damask Rose tobacco aromaticss according to claim 3, it is characterised in that described Step(1)In mixed solvent contained by ethyl alcohol be 20-30 mass parts, propylene glycol is 10-20 mass parts, water is:40-60 mass Part.
5. the preparation method of a kind of Damask Rose tobacco aromaticss according to claim 3, it is characterised in that described Step(4)In Dm301 types macroporous absorbent resin with after 95% ethyl alcohol soaked overnight, after distilled water flushing to no ethanol flavor, then 4h is impregnated with the solution of 4%NaOH, with distilled water flushing to neutrality;4h finally is impregnated with 4% HCl solution, uses distilled water flushing To neutrality, dress column is spare, and cylinder specification is 10cm × 60cm.
6. a kind of application of Damask Rose tobacco aromaticss, which is characterized in that wherein by cigarette shreds 0.03wt%- 0.1wt% weighs Damask Rose tobacco aromaticss, and after being dissolved with 30wt% ethanol waters, spray is added in flue-cured tobacco pipe tobacco.
CN201810038174.5A 2018-01-16 2018-01-16 A kind of Damask Rose tobacco aromaticss and its preparation method and application Pending CN108102787A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102851118A (en) * 2011-06-27 2013-01-02 湖北中烟工业有限责任公司 Extraction process of rose essence for cigarette
CN104171157A (en) * 2014-09-10 2014-12-03 嘉兴市得百科新材料科技有限公司 Green tea extract as well as preparation method and application thereof
CN105087160A (en) * 2015-08-20 2015-11-25 嘉兴景程生物科技有限公司 Camomile tobacco flavor as well as preparation method and application thereof
CN105105320A (en) * 2015-08-20 2015-12-02 嘉兴景程生物科技有限公司 Moisture preserving and aroma enhancing tobacco flavor, and preparation method and application thereof
CN105707973A (en) * 2014-09-10 2016-06-29 邹玉华 Green tea extract and preparation method thereof
CN105767326A (en) * 2014-09-10 2016-07-20 邹玉华 Green tea extract and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102851118A (en) * 2011-06-27 2013-01-02 湖北中烟工业有限责任公司 Extraction process of rose essence for cigarette
CN104171157A (en) * 2014-09-10 2014-12-03 嘉兴市得百科新材料科技有限公司 Green tea extract as well as preparation method and application thereof
CN105707973A (en) * 2014-09-10 2016-06-29 邹玉华 Green tea extract and preparation method thereof
CN105767326A (en) * 2014-09-10 2016-07-20 邹玉华 Green tea extract and preparation method thereof
CN105087160A (en) * 2015-08-20 2015-11-25 嘉兴景程生物科技有限公司 Camomile tobacco flavor as well as preparation method and application thereof
CN105105320A (en) * 2015-08-20 2015-12-02 嘉兴景程生物科技有限公司 Moisture preserving and aroma enhancing tobacco flavor, and preparation method and application thereof

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