CN109330016A - A kind of Exocarpium Citri Grandis medicinal extract, preparation method and the application in cigarette - Google Patents
A kind of Exocarpium Citri Grandis medicinal extract, preparation method and the application in cigarette Download PDFInfo
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- CN109330016A CN109330016A CN201811350634.4A CN201811350634A CN109330016A CN 109330016 A CN109330016 A CN 109330016A CN 201811350634 A CN201811350634 A CN 201811350634A CN 109330016 A CN109330016 A CN 109330016A
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- exocarpium citri
- citri grandis
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention discloses the medicinal extract, preparation method and the application in cigarette of a kind of Exocarpium Citri Grandis, belong to natural perfume material preparation and cigarette applied technical field, the preparation method includes: 1) to crush: by Exocarpium Citri Grandis at 40-60 DEG C after drying, crushing, crosses 40-80 mesh, obtain Exocarpium Citri Grandis powder；2) extract: by Exocarpium Citri Grandis powder obtained in step 1) according to 1:(5-12) solid-to-liquid ratio be dissolved in the ethanol solution of 40-60%, after ultrasound, obtain Exocarpium Citri Grandis extract；3) be concentrated: by Exocarpium Citri Grandis extract that step 2 obtains with alcohol solvent be filtered, washed it is rear, be evaporated under reduced pressure under 35-50 DEG C, the vacuum degree of 50-100Pa, Exocarpium Citri Grandis medicinal extract.The Exocarpium Citri Grandis medicinal extract being prepared can be used as cigarette additive, increase the sweet sense of flue gas, improve flue gas comfort level, improves pleasant impression, keeps cigarette perfume finer and smoother soft, reduce the sense of discomfort generated in sucking process to throat, nasal cavity and oral cavity.
Description
Technical field
The invention belongs to natural perfume material preparation and cigarette applied technical fields, and in particular to a kind of medicinal extract of Exocarpium Citri Grandis, its
Preparation method and the application in cigarette.
Background technique
In recent years, as Chinese-style cigarette " lowering harm and decreasing coking " engineering deeply promotes, cigarette product is resulted in a certain extent
The loss of fragrance matter, the decline of sucking quality.In addition, smoker generally has the symptoms such as cough, abundant expectoration, bronchitis.Therefore,
Cigarette flavor amount, which how can be improved, reduce dry sensation and improve oral cavity and nasal cavity comfort becomes domestic cigarette research hair
The direction of exhibition.
Exocarpium Citri Grandis, also known as " Huajuhong ", " Huazhou dried orange peel ", " shaddock ped Exocarpium Citri Rubrum " etc. are rutaceae Citrus grandis or shaddock
Prematurity or maturescent dry outside rind, be important Chinese medicine.Exocarpium Citri Grandis has resolving sputum, cough-relieving, anti-inflammatory, sharp gas etc.
Effect, therefore, the product development of Exocarpium Citri Grandis are also like a raging fire, such as Exocarpium Citri Grandis productive cough cream, electuary, medicine materical crude slice.Usually utilize tradition
Extraction method, Maillard reaction method, supercritical extraction, biotechnology method process Exocarpium Citri Grandis, CN201110029217.1
Disclose it is a kind of using specific extraction agent to Chinese medicine Exocarpium Citri Grandis fruit, the preparation method for the positions such as spending to extract；
CN02114847.3 discloses a kind of Exocarpium Citri Grandis preparation and its production method, and Exocarpium Citri Grandis all-fruit powder is broken, by water extract one to
Three times, be collected simultaneously volatile oil, filtering, separation be condensed into medicinal extract, there are extraction process complexity, higher costs etc. for the above method
Defect.Ultrasonic extraction is the movement that material molecule is improved by cavitation, fuel factor and mechanism of ultrasonic wave etc.
Frequency and speed are conducive to the dissolution of substance, have the advantages that time saving, easy to operate, extraction yield is high.Therefore, in conjunction with tobacco
How industry production actual conditions quickly and effectively extract the effective component in Exocarpium Citri Grandis and are applied to seem especially in cigarette product
It is important.
Summary of the invention
The purpose of the present invention is to provide extraction medicinal extract, preparation method and the applications in cigarette of a kind of Exocarpium Citri Grandis.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of Exocarpium Citri Grandis medicinal extract, including following preparation step:
1) it crushes: taking the full fruit cleaning of Exocarpium Citri Grandis, slice, drying to constant weight (moisture content is 12 ± 1% at this time), crush, cross 40-80
Mesh obtains Exocarpium Citri Grandis powder；
2) extract: by Exocarpium Citri Grandis powder obtained in step 1) according to 1:(15-30) solid-liquid mass ratio be dissolved in extracting solution, surpass
After sound extracts 2 ~ 4h, filtering, merging filtrate；
3) it is centrifuged: the filtrate that step 2 is collected being centrifuged, supernatant is taken；
4) be concentrated: the supernatant that step 3) is obtained is concentrated, and obtains Exocarpium Citri Grandis medicinal extract.
Exocarpium Citri Grandis in the present invention is positive the full fruit of texturing Exocarpium Citri Rubrum.
Further, step 1) slice thickness 1-2mm, drying temperature are 40-60 DEG C, and drying time is 24~36h.
Further, ultrasonic wave extraction frequency 20-40Hz, 60-75 DEG C of extracting solution temperature, extracting solution are water or 70-90v%
Ethyl alcohol.
Further, centrifugal condition in step 3) are as follows: 2500 ~ 3500r/min of revolving speed, centrifugation time are 15~25min.
Further, 1-2h is concentrated at vacuum degree 80-100kPa and obtains Exocarpium Citri Grandis medicinal extract for extracting solution in step 4).
Exocarpium Citri Grandis medicinal extract made from above-mentioned preparation method, the Exocarpium Citri Grandis medicinal extract are divided into water according to the difference of extracting solution and extract
Exocarpium Citri Grandis medicinal extract and alcohol extracting Exocarpium Citri Grandis medicinal extract.
By the Exocarpium Citri Grandis medicinal extract Agilent7890A-5975C type gas chromatograph-mass spectrometer being prepared in step 4) (U.S.'s peace
Prompt Lun Science & technology Co., Ltd) and 400 nuclear magnetic resonance chemical analysers (VARIAN Oncology Systems) progress constituent analysis:
It was found that its ingredient mainly contains fructose (fructose), glucose (glucose), xylose (xylose), mannose
(mannose), the carbohydrates such as arabinose (arabinose), Sionit (sorbitol sugar) and sucrose (sucrose)
Compound, they are sweet substances, play improvement and modification cigarette flavor, increase sweet sense, have for increasing cigarette sweet moisture feeling
Directly act on；Linoleic acid (linoleiic acid), citric acid (citric acid), 2- acrylic acid (2-propenoic
Acid), pentadecanoic acid (pentadecanoic acid), certain herbaceous plants with big flowers acid (decanoic acid), palmitinic acid (palmitic acid)
Equal acid compounds, they are sour odour materials, can neutralize the alkaline matters such as the nicotine in pipe tobacco and flue gas well, make the flue gas be in
The effects of subacidity plays improvement mouthfeel, reduces cigarette irritation, cover cigarette foreign gas, increase throat's comfort；Limonene
(cinene), citral (citral), citric acid (citric acid), linalool (linalool), laurene (myrcene),
Sabinene (sabinen), firpene (pinene), cadinene (cadinene), elemene (elemene), germacrene
(germacrene), aurantiin (naringin), Rhoifolin (rhoifolin), Isomperatorin (isoimperatorin),
Bergaptol (bergaptol), marmin (maermin), meranzin (meranzin), different meranzin (isomeranzin),
6 ', 7 '-dihydroxy bergamot element (6 ', 7 '-dihydroxycitrate), 6- isopropoxy-ayapanin (6-
Isopromethoxy-7-methoxy coumarin), 5- hydroxyl -8- (3 '-methyl -2 '-cyclobutenyl) furocoumarin (5-
Hydroxy-8- (3 '-methyl-2 '-butenyl) furan coumarin), naringenin (naringenin), apiolin
(apigenin), Poncirus glycosides (poncirin), aurantiin (naringin), neohesperidin (neohesperidin), linalool
(linalool), cis- geraniol (cis-geraniol), methyl palmitate (methyl palmitate), p-cymene
(p-cymene), 4- methyl -2- ketone (4-methyl-2-hexanone), 4- ergosterol -3- ketone (4-ergosterol-3-
Ketone), 4- stigmastene -3- ketone (4-bean sterene-3-ketone), 2- acrylic acid (2-propenoic acid), two
Phenylate (diphenyl oxide), benzaldehyde (benzaldehyde), certain herbaceous plants with big flowers sour (decanoic acid), orange geranyl acetate
(geranial acetate), pentadecanoic acid (pentadecanoic acid), palmitinic acid (palmitic acid), linoleic acid
Organic compounds such as (linoleiic acid) have feature breath compound, play improve fragrance quality and quantity, coordinate cigarette perfume,
Increase sense organ comfort level, improve the effect for inhaling taste and pleasant impression.Due to the presence of these acidic materials, sweet substance, flavor matter,
Enable the alkaline matters such as the nicotine for adding that the medicinal extract is neutralized well in pipe tobacco and flue gas, makes flue gas in subacidity, and play
Improve mouthfeel, reduce cigarette irritation, cover cigarette foreign gas, increases throat's comfort.
Exocarpium Citri Grandis medicinal extract can be applied in production of cigarettes as cigarette additive, and concrete application is divided into two aspects:
On the one hand, Exocarpium Citri Grandis medicinal extract is applied in the charging of piece cigarette, mainly improvement mouthfeel, specific steps are as follows: by medicinal extract, the third two
Alcohol, pure water are mixed according to 2 ︰ (3-5) ︰ (5-8) mass ratio, and additive feed liquid is obtained after mixing, additive feed liquid is sprayed on
On piece cigarette, additive feed liquid accounts for the 0.05-0.20% of piece cigarette weight；The more preferable water of medicinal extract extracts Exocarpium Citri Grandis medicinal extract.
On the other hand, Exocarpium Citri Grandis medicinal extract is applied on cigarette paper, and mainly enhancing cigarette flavor is rich, specific steps
Are as follows: by medicinal extract, Glycerin, mixed triester with caprylic acid capric acid, 70-90v% ethyl alcohol, according to 1 ︰, (2-4) ︰ (4-8) is mixed, and is mixed into coating spice liquid, is being rolled up
It will be coated on spice liquid even spread to cigarette paper in cigarette paper production process, up to Exocarpium Citri Grandis flavored type cigarette paper after drying, apply
For layer with a thickness of 0 .3-0.8 μm, coating weight is 0 .1-0.5g/m2；The more preferable alcohol extracting Exocarpium Citri Grandis medicinal extract of medicinal extract.
The utility model has the advantages that
(1) low in cost: the present invention has abandoned traditional tobacco aromaticss and has had drawn from the thinking inertias of rare animals and plants, select it is inexpensive easily
, Exocarpium Citri Grandis be raw material, not will increase the production cost of cigarette；
(2) simple process: it is of the present invention separation, centrifugation, concentration etc. processes, be not necessarily to large-scale instrument and equipment and expensive reagent,
It is easy to operate, it is easily controllable；
(3) efficiency is higher: the present invention uses ultrasonic wave extraction, time saving, easy to operate, recovery rate is high；
(4) significant effect: medicinal extract produced by the present invention includes sweet taste, tart flavour, causes fragrant and pharmacological property substance, is added in cigarette, can be with
Increase the sweet sense of flue gas well, improve flue gas comfort level, improve pleasant impression, keep cigarette perfume finer and smoother soft, reduces in sucking process
The sense of discomfort that throat generates, is suitable for the additive of cigarette.
Specific embodiment
Technical solution of the present invention is described in further detail below with reference to embodiment, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of preparation method of Exocarpium Citri Grandis medicinal extract, comprising the following steps:
1) it pre-processes: the full fruit of Exocarpium Citri Grandis being taken to wash with water only, slice, slice thickness 1mm is put into baking oven, and drying temperature is
40 DEG C, drying time about for 24 hours, carries out continuous dehumidifying in drying course, is dried to moisture content natural cooling in 12 ± 1%, baking oven,
It takes out, is then crushed with high speed Universal pulverizer grinder, cross 40 meshes, obtain Exocarpium Citri Grandis powder, the purpose that pulverizes and sieves is to make
The granularity of Exocarpium Citri Grandis powder is as thin as possible, convenient for the high efficiency extraction of wherein effective component.
2) ultrasonic wave extraction: taking Exocarpium Citri Grandis powder in 200g step 1), and wherein 100g is extracted three times with 500mL water, mentions every time
Liquid temperature 60 C is taken, through 20Hz ultrasonic wave extraction 4h, filtering, merging filtrate obtains aqueous extract；500mL90v% second is added in 100g
Alcohol extracting three times, every time through 40Hz ultrasonic wave extraction 4h, is filtered, merging filtrate obtains ethanol extract；
3) it is centrifuged: the filtrate collected in step 2 being centrifuged respectively using tube centrifuge, takes supernatant, parameter of noncentricity is
2500 r/min are centrifuged 15min, take supernatant；
4) it is concentrated under reduced pressure: taking supernatant in step 3), 1h is concentrated at vacuum degree 80kPa with Rotary Evaporators, obtains water extractionization
Exocarpium Citri Rubrum medicinal extract and alcohol extracting Exocarpium Citri Grandis medicinal extract；
5) water made from step 4) charging application: is extracted into Exocarpium Citri Grandis medicinal extract and propylene glycol and distilled water according to 2 ︰, 5 ︰, 8 mass ratio
Example mixing, obtains additive feed liquid, additive feed liquid is sprayed on piece cigarette, additive feed liquid accounts for piece cigarette weight after mixing
0.05-0.20%, according to normal production technology cigarette at cigarette, and (Bright Yellow brand is a certain in the cigarette without Exocarpium Citri Grandis medicinal extract
Class cigarette) it compares and smokes panel test, as a result as follows:
1 smoking property of cigarette sensory effects of table
From the smoking result of table 1: Exocarpium Citri Grandis medicinal extract of the present invention improve significantly mouthfeel and modify flue gas effect.Feed liquid
Applied amount is within the scope of 0.05-0.15%, and the sweet degree of mouthfeel increases, and dry sensation reduces, and throat's comfort improves, makes up well
The deficiencies of drying of cigarette smoke, stimulation, but after feed liquid applied amount reaches 0.15%, aroma quality is deteriorated, miscellaneous gas highlights, strength
Become larger big, it is therefore proposed that dosage: 0.05-0.15%.
6) cigarette paper application:
Alcohol extracting Exocarpium Citri Grandis medicinal extract made from step 4) and Glycerin, mixed triester with caprylic acid capric acid, 70v% ethyl alcohol are mixed according to 1 ︰, 2 ︰, 6 ratio, mixed
Coating spice liquid is obtained after conjunction, will be coated on spice liquid even spread to cigarette paper in cigarette paper production process, is after dry
Exocarpium Citri Grandis flavored type cigarette paper is obtained, coating layer thickness is 0.3 μm, coating weight 0.2g/m2.According to normal production technology cigarette at cigarette
Branch, and compare and smoke panel test in the cigarette (a kind of cigarette of Bright Yellow brand) without Exocarpium Citri Grandis medicinal extract, it is as a result as follows:
2 Exocarpium Citri Grandis of table extracts medicinal extract cigarette paper flavoring smoking result
From the smoking result of table 2: being coated with that cigarette flavor made from the cigarette paper of Exocarpium Citri Grandis medicinal extract is rich to improve, pleasant impression
Become comfortable, there is no significant change in terms of irritation and miscellaneous gas.
Embodiment 2
A kind of preparation method of Exocarpium Citri Grandis medicinal extract, comprising the following steps:
1) it pre-processes: the full fruit of Exocarpium Citri Grandis being taken to wash with water only, slice, slice thickness 2mm is put into baking oven, and drying temperature is
60 DEG C, drying time about 30h, continuous dehumidifying is carried out in drying course, is dried to moisture content natural cooling in 12 ± 1%, baking oven,
It takes out, is then crushed with high speed Universal pulverizer grinder, cross 60 meshes, obtain Exocarpium Citri Grandis powder, the purpose that pulverizes and sieves is to make
The granularity of Exocarpium Citri Grandis powder is as thin as possible, convenient for the high efficiency extraction of wherein effective component；
2) ultrasonic wave extraction: taking Exocarpium Citri Grandis powder in 200g step 1), and wherein 100g is added water 700mL and extracts three times, extracts every time
When extracting solution temperature 70 C, through 30Hz ultrasonic wave extraction 4h, filtering；Merging filtrate obtains aqueous extract；80v% second is added in 100g
Alcohol 1000mL is extracted three times, every time through 35Hz ultrasonic wave extraction 4h, is filtered, merging filtrate obtains ethanol extract；
3) it is centrifuged: the filtrate collected in step 2 being centrifuged respectively using tube centrifuge, takes supernatant, parameter of noncentricity is
2000 r/min are centrifuged 25min, take supernatant；
4) it is concentrated under reduced pressure: taking supernatant in step 3), 2h is concentrated at vacuum degree 80kPa with Rotary Evaporators, obtains water extractionization
Exocarpium Citri Rubrum medicinal extract and alcohol extracting Exocarpium Citri Grandis medicinal extract.
Embodiment 3
A kind of preparation method of Exocarpium Citri Grandis medicinal extract, comprising the following steps:
1) it pre-processes: the full fruit of Exocarpium Citri Grandis being taken to wash with water only, slice, slice thickness 1.5mm is put into baking oven, drying temperature
It is 50 DEG C, time about 36h carries out continuous dehumidifying in drying course, is dried to moisture content natural cooling in 12 ± 1%, baking oven, takes
Out, it is then crushed with high speed Universal pulverizer grinder, crosses 80 meshes, obtain Exocarpium Citri Grandis powder, the purpose that pulverizes and sieves is making
The granularity of Exocarpium Citri Rubrum powder is as thin as possible, convenient for the high efficiency extraction of wherein effective component；
2) ultrasonic wave extraction: taking Exocarpium Citri Grandis powder in 200g step 1), and wherein 100g is added water 1000mL and extracts three times, extracts every time
When 75 DEG C of temperature of extracting solution, through 20Hz ultrasonic wave extraction 4h, filtering；Merging filtrate obtains aqueous extract；70v% second is added in 100g
Alcohol 800mL is extracted three times, every time through 30Hz ultrasonic wave extraction 4h, is filtered, merging filtrate obtains ethanol extract
3) it is centrifuged: the filtrate collected in step 2 being centrifuged respectively using tube centrifuge, takes supernatant, parameter of noncentricity is
3500 r/min are centrifuged 15min, take supernatant；
4) it is concentrated under reduced pressure: taking supernatant in step 3), 1h is concentrated at vacuum degree 100kPa with Rotary Evaporators, obtains water extractionization
Exocarpium Citri Rubrum medicinal extract and alcohol extracting Exocarpium Citri Grandis medicinal extract.
Claims (8)
1. a kind of preparation method of Exocarpium Citri Grandis medicinal extract, which is characterized in that including following preparation step:
1) it crushes: taking the full fruit cleaning of Exocarpium Citri Grandis, slice, drying to constant weight, crush, cross 40-80 mesh, obtain Exocarpium Citri Grandis powder；
2) extracting: by Exocarpium Citri Grandis powder obtained in step 1) according to 1g:(15-30) mass volume ratio of mL is dissolved in extracting solution
In, after 2 ~ 4h of ultrasonic extraction, filtering, merging filtrate；
3) it is centrifuged: the filtrate that step 2 is collected being centrifuged, supernatant is taken；
4) be concentrated: the supernatant that step 3) is obtained is concentrated, and obtains Exocarpium Citri Grandis medicinal extract.
2. the preparation method of Exocarpium Citri Grandis medicinal extract as described in claim 1, which is characterized in that step 1) 1~2mm of slice thickness is done
Dry temperature is 40-60 DEG C, and drying time is 24~36h.
3. the preparation method of Exocarpium Citri Grandis medicinal extract as described in claim 1, which is characterized in that ultrasonic condition described in step 2 are as follows:
Ultrasonic wave extraction frequency 20-40Hz, 60-70 DEG C of extracting solution temperature, extracting solution are water or 70-90v% ethyl alcohol.
4. the preparation method of Exocarpium Citri Grandis medicinal extract as described in claim 1, which is characterized in that centrifugal condition in step 3) are as follows: revolving speed
2500~3500r/min, centrifugation time are 15~25min.
5. the preparation method of Exocarpium Citri Grandis medicinal extract as described in claim 1, which is characterized in that extracting solution is in vacuum degree in step 4)
1-2h is concentrated under 80-100kPa and obtains Exocarpium Citri Grandis medicinal extract.
6. obtaining Exocarpium Citri Grandis medicinal extract using any preparation method of claim 1-5.
7. application of the Exocarpium Citri Grandis medicinal extract as piece cigarette additive described in claim 6, which is characterized in that specific steps are as follows: will soak
Cream, propylene glycol, distilled water are mixed according to 2 ︰ (3-5) ︰ (5-8) mass ratio, additive feed liquid are obtained after mixing, by additive feed liquid
It is sprayed on piece cigarette, additive feed liquid accounts for the 0.05-0.20% of piece cigarette weight.
8. application of the Exocarpium Citri Grandis medicinal extract described in claim 6 as cigarette paper coating fragrance, which is characterized in that by medicinal extract, the pungent last of the ten Heavenly stems
(2-4) ︰ (4-8) is mixed, and coating spice liquid is mixed into, in cigarette paper production process according to: 1 ︰ for acid glyceride, 70-90v% ethyl alcohol
Middle to be coated on spice liquid even spread to cigarette paper, up to Exocarpium Citri Grandis flavored type cigarette paper after drying, coating layer thickness is 0 .3-
0.8 μm, coating weight 0.1-0.5g/m2。
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| CN201811350634.4A CN109330016A (en) | 2018-11-14 | 2018-11-14 | A kind of Exocarpium Citri Grandis medicinal extract, preparation method and the application in cigarette |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114568738A (en) * | 2021-12-07 | 2022-06-03 | 云南恒罡科技有限公司 | Low-temperature heating non-combustible product prepared from flexible carbonized exocarpium citri rubrum particles and application |
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| CN114568738B (en) * | 2021-12-07 | 2023-03-14 | 云南恒罡科技有限公司 | Low-temperature heating non-combustible product prepared from flexible carbonized exocarpium citri rubrum particles and application thereof |
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Application publication date: 20190215 |