CN108330000A - A kind of dragon's paw carpopodium extract and its preparation method and application - Google Patents
A kind of dragon's paw carpopodium extract and its preparation method and application Download PDFInfo
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- CN108330000A CN108330000A CN201810312199.XA CN201810312199A CN108330000A CN 108330000 A CN108330000 A CN 108330000A CN 201810312199 A CN201810312199 A CN 201810312199A CN 108330000 A CN108330000 A CN 108330000A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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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
- A24B15/241—Extraction of specific substances
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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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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A kind of dragon's paw carpopodium extract of present invention offer and its preparation method and application, the preparation method includes：Extracting solution is obtained as extractant extraction dragon's paw carpopodium using ethanol water or water；Filtering, separation, obtain the supernatant liquor of extracting solution；It concentrates supernatant liquor and obtains dragon's paw carpopodium extract.Dragon's paw carpopodium extract in the application is used as the suction quality that natural tobacco additive is used to improve tobacco material such as stem, thin slice or tobacco leaf etc., its can enrich with enrichment flue gas, promote aroma quality and perfume quantity, reduce the irritation and dry sensation of flue gas, make the soft exquisiteness of flue gas, covers miscellaneous gas.
Description
Technical field
The present invention relates to a kind of tobacco additive agents and preparation method thereof, and tobacco original can be effectively improved more particularly to one kind
Natural baccy additive of the suction quality of material and preparation method thereof.
Background technology
Honey raisin tree also known as papaw, trifoliate orange Dulcis, dragon's paw, are Rhamnaceae, and spray, the spire back side, petiole and rachis just have
Pubescence, after fall off.Blade ellipticity is oval, width egg shape or heart shaped are oval.Carpopodium glucose containing volume and potassium malate, through frost
Sweet tea afterwards can be eaten raw or make wine；The hardness of wood is moderate, and texture is beautiful, for building and the material of furniture processed and artistic handicraft etc..Distribution
Henan, Shaanxi, Longnan of Gansu Province, Jiangxi, Anhui, Zhejiang, Guangdong, Fujian, Hubei, Hunan etc..Fruit morphology claims like ten thousand characters
It is papaw tree that it, which is set,.Fruit is well-done raw-eaten, and pulp is starched more, and no fruit stone, seed is exposed except pulp, and it is slightly sweet that taste starches sweet tea
It is puckery, it can also cook soup, soup taste uniqueness mellowness.Xiang Jinle was the 2nd phase in 2015《Chinese Forest by-product and speciality》In deliver《Fruit stalk of Hovenia dulcis THunb
Trophic function and processing and utilization》Described in trifoliate orange Dulcis carpopodium edible and reduced sugar (glucose and fructose), amino acid, albumen
Matter, organic acid (malic acid, citric acid, fumaric acid etc.), vitamin (vitamin C, vitamin B1, vitamin B2, carrotene),
The content of polyphenols etc. is higher；Its nutrient constituents of fruit is abundant, has certain healthcare function, can cook fruit wine, fruit juice, fruit
Vinegar etc., son can reducing fever and causing diuresis, cough-relieving relieving restlessness, Antialcoholic liver-protecting.
Lack the patent that honey raisin tree carpopodium is promoted to tobacco suction quality for cigarette in the prior art.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of dragon's paw carpopodium extract and its
Preparation method and purposes, for solving the problems of the prior art.
In order to achieve the above objects and other related objects, the present invention obtains by the following technical programs.
The present invention provides a kind of preparation method of dragon's paw carpopodium extract, includes the following steps：
1) ethanol water or water is used to obtain extracting solution as extractant extraction dragon's paw carpopodium；
2) it filters, detach, obtain the supernatant liquor of extracting solution；
3) concentration supernatant liquor obtains dragon's paw carpopodium extract.
Dragon's paw carpopodium in the application is to use to spontaneously dry, and remove impurity and the shrivelled part for having worm-eaten of going mouldy.
The concentration of ethanol water in step 1), can be selected according to actual conditions.Preferably, ethyl alcohol in step 1)
The a concentration of of aqueous solution is no more than 95wt%.
Preferably, in step 1), the solid-liquid ratio of dragon's paw carpopodium and ethanol water is 1g：(5~9) ml.
Preferably, in step 1), the solid-liquid ratio of dragon's paw carpopodium and water is 1g：(5~9) ml.
Preferably, extracting mode is the refluxing extraction at 60~100 DEG C in step 1).It is highly preferred that reflux extracting time
For 1~6h.It is highly preferred that can first be impregnated before refluxing extraction.Soaking time is not less than 12h.
Preferably, in step 1) extracting mode can also at 40 DEG C~80 DEG C ultrasonic extraction.It is highly preferred that ultrasonic extraction
Time be (1~6) h.
Preferably, when ultrasonic extraction, power is 300~350w, and frequency is 30~40kHz.
Preferably, filtering is filtered using 40 mesh filter screens in step 2).Filtrate is obtained after filtering, filtrate obtains through separation
Supernatant liquor.Carpopodium slag is removed using strainer filtering, still contains insoluble matter in filtrate.
Preferably, separation uses centrifugation in step 2).After being centrifuged, insoluble matter is settled down to lower layer, by dividing
From acquisition supernatant liquor.Centrifuge is used in centrifugation, the rotating speed of centrifuge is 1500~3000rpm.
Preferably, in step 3), concentration supernatant liquor to density is 1.15~1.35g/cm3.Under this density, acquisition
Dragon's paw carpopodium extract is easy to preserve, and in final use is easy to be diluted easy to use.
Preferably, in step 3), concentrated by rotary evaporation under supernatant liquor is (0.01~0.1) MPa in (40~70) DEG C, vacuum degree
Obtain dragon's paw carpopodium extract.
The invention also discloses a kind of dragon's paw carpopodium extracts to be prepared by preparation method described above.
The invention also discloses dragon's paw carpopodium extract described above as cigarette additive for improving tobacco material
The purposes of suction quality.
Preferably, tobacco material described herein includes stem, flue-cured tobacco pipe tobacco, thin slice and tobacco leaf.
Preferably, the purposes is that the dragon's paw carpopodium extract is dissolved in ethanol water to form cigarette additive spray
It spills or is coated on the tobacco material.It is highly preferred that the mass ratio of the dragon's paw carpopodium extract and ethanol water be 2~
10wt%.Preferably, the concentration of the ethanol water is not less than 25wt%.
Preferably, the additive amount of the dragon's paw carpopodium extract is 0.01~0.15wt% of the tobacco material quality.
It is highly preferred that the additive amount of the dragon's paw carpopodium extract is 0.01~0.1wt% of the tobacco material quality.Preferably,
The additive amount of the dragon's paw carpopodium extract is 0.02~0.05wt% of the tobacco material quality, 0.03~0.06wt%,
0.04~0.06wt%, 0.05~0.1wt%, 0.02~0.08wt% or 0.03~0.07wt%.
This application discloses a kind of natural baccy additives and preparation method thereof, and preparation method is simple and practicable and effective,
Suitable in heavy industrialization and safety in production, this simple for process easily operated, solvent for use is cheap and easy to get, Bu Huizao
At environmental pollution, miscellaneous gas will not be introduced.It uses the carpopodium of the dragon's paw (honey raisin tree) with safety, edibility as raw material, leads to
Certain extraction concentration technique process is crossed, the natural tobacco additive that can be used for improving tobacco material suction quality is made.Due to
Containing a large amount of glucose, fructose etc. in fresh fruit or dry fruit inspissated juice, also contain polysaccharide constituents, these carbohydrates and amino acid
Reaction product is in the richness of modification flue gas, and protrusion cigarette style aspect is with more superiority.This natural tobacco additive is used
In the suction quality for improving tobacco material such as stem, thin slice or tobacco leaf etc., enrich and enrichment flue gas, promotion aroma quality and fragrance
Amount, reduces the irritation and dry sensation of flue gas so that the soft exquisiteness of flue gas covers miscellaneous gas.
Description of the drawings
Fig. 1 is that the GC-MS analyses total ion current figure of extracting solution obtained by different ethanol concentration solvent extraction compares
Top-down curve represents successively in wherein Fig. 1：Make using water as extractant, with the ethanol water of 15wt%
Ethanol water of the ethanol water as extractant, using 50wt% for extractant, using 30wt% as extractant, with
The ethanol water of 70wt% is as extractant.
Fig. 2 is that the pyrolysis gas chromatography mass spectrometry of extracting solution obtained by different ethanol concentration solvent extraction analyzes total ion current figure ratio
Compared with
Top-down curve represents successively in wherein Fig. 2：Make using water as extractant, with the ethanol water of 15wt%
For ethanol water second as extractant, 70wt% of the ethanol water as extractant, 50wt% of extractant, 30wt%
Alcohol solution is as extractant.
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this explanations by particular specific embodiment below
Content disclosed by book understands other advantages and effect of the present invention easily.
Before further describing the specific embodiments of the present invention, it should be appreciated that protection scope of the present invention is not limited to down
State specific specific embodiment；It is also understood that the term used in the embodiment of the present invention is specific specific in order to describe
Embodiment, the protection domain being not intended to be limiting of the invention.The test method of actual conditions is not specified in the following example,
Usually according to normal condition, or according to the condition proposed by each manufacturer.
When embodiment provides numberical range, it should be appreciated that except non-present invention is otherwise noted, two ends of each numberical range
Any one numerical value can be selected between point and two endpoints.Unless otherwise defined, in the present invention all technologies for using and
Scientific terminology is identical as the normally understood meaning of those skilled in the art of the present technique.Except used in embodiment specific method, equipment,
Outside material, the record according to those skilled in the art to the grasp of the prior art and the present invention can also use and this
Any method, equipment and the material of the similar or equivalent prior art of method, equipment described in inventive embodiments, material come real
The existing present invention.
Dragon's paw carpopodium in the embodiment of the present application is to use to spontaneously dry, and remove impurity and the shrivelled portion for having worm-eaten of going mouldy
Point.
Embodiment 1
Dragon's paw carpopodium 300g is taken, is impregnated for 24 hours with 2400ml water, then heating and refluxing extraction 4h at 80 DEG C again.
Extraction terminates postcooling, and the filtering of 40 mesh filter screens is used in combination to obtain filtrate, and filtrate is separated by solid-liquid separation through centrifuge, is collected
Supernatant liquor；
Rotary evaporation under the conditions of 70 DEG C, vacuum degree 0.01MPa is concentrated to give dragon's paw stalk extract 119g.
Embodiment 2
It takes dragon's paw carpopodium 300g, is added in the ethanol water of a concentration of 50wt% of 2100ml, then heat at 60 DEG C again
Refluxing extraction 6h.
Extraction terminates postcooling, and the filtering of 40 mesh filter screens is used in combination to obtain filtrate, and filtrate is separated by solid-liquid separation through centrifuge, is collected
Supernatant liquor；
Rotary evaporation under the conditions of 45 DEG C, vacuum degree 0.02MPa is concentrated to give dragon's paw stalk extract 108g.
Embodiment 3
It takes dragon's paw carpopodium 300g, is added in the ethanol water of a concentration of 70wt% of 1500ml, then heat at 80 DEG C again
Refluxing extraction 2h.
Extraction terminates postcooling, and the filtering of 40 mesh filter screens is used in combination to obtain filtrate, and filtrate is separated by solid-liquid separation through centrifuge, is collected
Supernatant liquor；
Rotary evaporation under the conditions of 40 DEG C, vacuum degree 0.04MPa is concentrated to give dragon's paw stalk extract 95g.
Embodiment 4
Dragon's paw carpopodium 300g is taken, is added in the ethanol water of a concentration of 50wt% of 1800ml, it is then ultrasonic at 60 DEG C
Extract 1h.Ultrasonic power 320w, frequency 37kHz.
Extraction terminates postcooling, and the filtering of 40 mesh filter screens is used in combination to obtain filtrate, and filtrate is separated by solid-liquid separation through centrifuge, is collected
Supernatant liquor；
Rotary evaporation under the conditions of 45 DEG C, vacuum degree 0.02MPa is concentrated to give dragon's paw stalk extract 110g.
Embodiment 5
Dragon's paw carpopodium 300g is taken, is added in the ethanol water of a concentration of 70wt% of 1800ml, it is then ultrasonic at 50 DEG C
Extract 75min.Ultrasonic power 300w, frequency 37kHz.
Extraction terminates postcooling, and the filtering of 40 mesh filter screens is used in combination to obtain filtrate, and filtrate is separated by solid-liquid separation through centrifuge, is collected
Supernatant liquor；
Rotary evaporation under the conditions of 40 DEG C, vacuum degree 0.04MPa is concentrated to give dragon's paw stalk extract 112g.
Embodiment 6
It is with a concentration of 75wt% ethanol waters dissolved dilution by the dragon's paw carpopodium extract obtained in embodiment 1
2wt% concentration, it is spare.It is sprayed onto on flue-cured tobacco pipe tobacco by the 0.01% of pipe tobacco weight, 0.05%, 0.1% respectively, rolls into cigarette,
It after climatic chamber equilibrium water conten 48h, smokes panel test, determines that 0.05% additive amount suction effect is preferable through smokeing panel test.
Embodiment 7
With the ethanol water dissolved dilution of a concentration of 75wt% it is 5wt% by 2 gained dragon's paw carpopodium extract of embodiment
Concentration, it is spare.It is sprayed onto on flue-cured tobacco pipe tobacco by the 0.05% of pipe tobacco weight, 0.08%, 0.1% respectively, cigarette is rolled into, in constant temperature
It after constant humidity cabinet equilibrium water conten 48h, smokes panel test, determines that 0.08% additive amount suction effect is preferable through smokeing panel test.
Embodiment 8
With the ethanol water dissolved dilution of a concentration of 75wt% it is 10wt% by 3 gained dragon's paw carpopodium extract of embodiment
Concentration, it is spare.It is sprayed onto on flue-cured tobacco pipe tobacco by the 0.05% of pipe tobacco weight, 0.1%, 0.15% respectively, cigarette is rolled into, in constant temperature
It after constant humidity cabinet equilibrium water conten 48h, smokes panel test, determines that 0.1% additive amount suction effect is preferable through smokeing panel test.
Embodiment 9
With the ethanol water dissolved dilution of a concentration of 75wt% it is 5wt% by 4 gained dragon's paw carpopodium extract of embodiment
Concentration, it is spare.It is sprayed onto on flue-cured tobacco pipe tobacco by the 0.05% of pipe tobacco weight, 0.08%, 0.1% respectively, cigarette is rolled into, in constant temperature
It after constant humidity cabinet equilibrium water conten 48h, smokes panel test, determines that 0.08% additive amount suction effect is preferable through smokeing panel test.
Embodiment 10
With the ethanol water dissolved dilution of a concentration of 75wt% it is 10wt% by 5 gained dragon's paw carpopodium extract of embodiment
Concentration, it is spare.It is sprayed onto on flue-cured tobacco pipe tobacco by the 0.05% of pipe tobacco weight, 0.1%, 0.15% respectively, cigarette is rolled into, in constant temperature
It after constant humidity cabinet equilibrium water conten 48h, smokes panel test, determines that 0.1% additive amount suction effect is preferable through smokeing panel test.
Embodiment 11
The present embodiment mainly analyzes the flavor substance of dragon's paw carpopodium extract.Mainly include the following steps：
1) it pre-processes：The extracting solution obtained as extractant using ethanol water removes second before carrying out liquid-liquid extraction
Alcohol, the mode for removing ethyl alcohol are to be rotated under 35~45 DEG C, the vacuum degree of 0.03MPa or so；
2) liquid-liquid extraction：Liquid-liquid extraction, extraction are carried out using organic solvent to the preprocessed extracting solution for being free of ethyl alcohol
Liquid is concentrated to be packed into sample injection bottle to after 1ml, and flavor substance analysis is carried out using gas chromatography-mass spectrometry instrument；
The organic solvent is one or more in n-hexane, pentane, ether and dichloromethane；
3) GC-MS is analyzed：
Middle polarity column or low-pole column can be selected in chromatographic column；Using temperature programming：50 DEG C of holding 1min, with 3 DEG C/min
150 DEG C are raised to, 5min is kept, then 250 DEG C are raised to 5 DEG C/min, keeps 10min.Injector temperature：250.0℃；Carrier gas：It is high
Pure helium (99.999%), column flow rate：1.2mL/min；Sample size：1 μ L, split ratio：10:1
Mass Spectrometry Conditions:
Electron bombardment (EI) ion source；Ionizing energy：70eV；Interface temperature：280℃；Ion source temperature：230℃；Level Four
Bar temperature：150℃；Scanning quality range：35~450u.
Qualitative and semi-quantitative method:
Pass through NIST11, WILEY275 and Flavor2 mass spectrum library searching, selection matching score>80 and peak area normalize
The component that percentage comes top ten is listed in the result；The percentage contents of each component are calculated with areas of peak normalization method.
4) interpretation of result
GC/MS methods, which are primarily adapted for use in analysis, has certain volatile substance, therefore this test result only illustrates to extract
The case where volatilization in liquid and half volatile substance, it cannot be said that the case where nonvolatile matter in bright extracting solution.
It can be seen that the aroma compound that different determining alcohol extracting solutions are included is differentiated from figure, determining alcohol is got over
Height, volatilization semi-volatile compounds number contained in extracting solution are more.Wind in aqueous solution and low determining alcohol solvent extraction liquid
Taste compound appearance time is early, and the compound in high concentration ethanol solvent extraction liquid has appearance in each period, posterior segment
The compound of chromatographic column is flowed out based on fatty acid, esters and phytosterol, plant bases.95% extract is contained due to ethyl alcohol
Amount is high, leads to the water-soluble substances such as its sugar, amino acid, the albumen that cannot fully extract in dragon's paw carpopodium, recovery rate is too low, therefore
The extracting solution of the concentration does not do parallel comparison (including liquid-liquid extraction-GC/MS analyses and cracking point with the extracting solution of other determining alcohols
Analysis), only do the aroma compound analysis of its own.
The difference of appraisable main compound in the extracting solution of the simple more different determining alcohol solvents of table 1.
GC-MS analysis result of 1 water of table as extractant
GC-MS analysis result of the 2 15wt% ethyl alcohol of table as extractant
GC-MS analysis result of the 3 30wt% ethanol waters of table as extractant
GC-MS analysis result of the ethanol water of 4 50wt% of table as extractant
GC-MS analysis result of the 5 70wt% ethanol waters of table as extractant
GC-MS analysis result of the ethanol water of 6 95wt% of table as extractant
| Chinese | Molecular formula | CAS | Peak area normalizes |
| Palmitic acid | C16H32O2 | 57-10-3 | 5.88% |
| (Z, Z) -9,12- linoleic acid | C18H32O2 | 60-33-3 | 4.86% |
| E-9- oleic acid | C18H34O2 | 112-79-8 | 4.51% |
| - 3,5 hydroxyl -6- methyl -4H- pyrans -4- ketone of 2,3- dihydros | C6H8O4 | 28564-83-2 | 3.84% |
| 5- hydroxyl furfurals | C6H6O3 | 67-47-0 | 2.50% |
| Stearic acid | C18H36O2 | 57-11-4 | 1.31% |
| Pyrrolidines | C4H9N | 42403-25-8 | 1.20% |
| 1,2- cyclopentanediones | C5H6O2 | 3008-40-0 | 1.09% |
| Furfural | C5H4O2 | 98-01-1 | 0.95% |
| 2- furancarboxylic acid hydrazides | C5H6N2O2 | 3326-71-4 | 0.95% |
From above-mentioned 6 tables it can be seen that the main flavor compound contained by the extracting solution of different determining alcohol solvents obviously not
Together, high determining alcohol extracting solution contains long-chain fat acids, esters, alkaloids, long chain alkanol substance, these substances are being burnt and sucked
There is more significant impact to flue gas in the process.
The extractant of low determining alcohol can then extract more water-soluble, non-volatile substances, (also such as glucide
Raw sugar, oligosaccharide and polysaccharide), protein matter etc., these substances can not detect on gas-chromatography.
Embodiment 12
The present embodiment is the pyrolysis product analysis experiment of dragon's paw carpopodium extract.
Condition of simulation when burning and sucking, cracking atmosphere are oxygen-nitrogen mixture (oxygen and nitrogen by volume 9：91 mixing), it splits
Solve temperature program：300 DEG C of initial temperature keeps 5s, rises to 900 DEG C with 30 DEG C/s, keeps 5s.The product formed is cracked through nitrogen
Purging enters cold-trap, and condenser temperature rises to 280 DEG C by -60 DEG C in 5min, is desorbed, while sample introduction is passed through to gas-chromatography
Enter Mass Spectrometer Method after chromatography post separation.
Chromatographic condition
Chromatographic column HP-5MS (250 μm of 30m x, 0.25 μm of x)；250 DEG C of injector temperature, transmission line temperature：280℃；
Carrier gas：He gas；Shunt mode, split ratio 10:1；Column flow rate 1mL/min；Dottle pin purge flow rate 3mL/min；Temperature program：40℃
It is kept for 3 minutes, then 10 DEG C/min to 240 DEG C, is then kept for 15 minutes for 20 DEG C/min to 280 DEG C.
MS acquisition parameters
Electron bombardment (EI) ion source；Ionizing energy：70eV；Interface temperature：280℃；Full scan mass number range：29-
450；Ion source temperature：230℃；Quadrupole rod temperature:150℃；Solvent delay:1.50 minute.
Qualitative and semi-quantitative method
Pass through NIST11, WILEY275 and Flavor2 mass spectrum library searching, selection matching score>80 and peak area normalize
The component that percentage comes top ten is listed in the result；The percentage contents of each component are calculated with areas of peak normalization method.
As can be seen from Figure 2 with the raising of determining alcohol, the pyrolysis product type of extracting solution is also increasing, this with smoke panel test
Performance be closely related.Contain more water-soluble substances in the extracting solution of low determining alcohol, these substances include reduced sugar, two
Sugar, oligosaccharide, water-soluble polysaccharide, amino acid, protein, pectin etc. have good contribution in concentration appropriate to flue gas,
Then negatively correlated with suction quality when but if the amount of protein and pectin is larger.Contain more water in the extracting solution of high determining alcohol
Insoluble substance, such as long-chain fat acids, esters, sterols, polyphenols, these substances also have flue gas good
Effect.Which kind of extractant needs is specifically selected to be determined according to target is used.
Table 6a and table 6b lists the gas phase of extracting solution pyrolysis product under the conditions of simulation is burnt and sucked of different determining alcohol solvents
Chromatograph-mass spectrometer coupling analysis as a result, only listing matching score>80 and peak area normalization percentage come the group of top ten
Point.
Table 6a
Table 6b
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of preparation method of dragon's paw carpopodium extract, includes the following steps：
1) ethanol water or water is used to obtain extracting solution as extractant extraction dragon's paw carpopodium；
2) it filters, detach, obtain the supernatant liquor of extracting solution；
3) concentration supernatant liquor obtains dragon's paw carpopodium extract.
2. preparation method according to claim 1, which is characterized in that in step 1), dragon's paw carpopodium and ethanol water
Solid-liquid ratio is 1g：In (5~9) ml or step 1), the solid-liquid ratio of dragon's paw carpopodium and water is 1g：(5~9) ml.
3. preparation method according to claim 1, which is characterized in that extracting mode is at 60~100 DEG C in step 1)
Refluxing extraction or the ultrasonic extraction at 40 DEG C~80 DEG C.
4. preparation method according to claim 1, which is characterized in that filtering was carried out using 40 mesh filter screens in step 2)
Filter.
5. preparation method according to claim 1, which is characterized in that in step 3), supernatant liquor is in (40~70) DEG C, true
Reciprocal of duty cycle is that concentrated by rotary evaporation obtains dragon's paw carpopodium extract under (0.01~0.1) MPa.
6. a kind of dragon's paw carpopodium extract, which is characterized in that the dragon's paw carpopodium extract is by including that Claims 1 to 5 such as is appointed
Preparation method described in one prepares.
7. a kind of dragon's paw carpopodium extract as claimed in claim 6 is used to improve the suction of tobacco material as cigarette additive
The purposes of quality.
8. purposes according to claim 7, which is characterized in that the tobacco material include stem, flue-cured tobacco pipe tobacco, thin slice and
Tobacco leaf.
9. purposes according to claim 7, which is characterized in that the purposes is that the dragon's paw carpopodium extract is dissolved in second
Cigarette additive sprinkling is formed in alcohol solution or is coated on the tobacco material.
10. purposes according to claim 9, which is characterized in that the matter of the dragon's paw carpopodium extract and ethanol water
Amount is than being 2~10wt%.
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Cited By (1)
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| CN113457209A (en) * | 2021-08-20 | 2021-10-01 | 上海烟草集团有限责任公司 | Preparation method and application of dried orange peel spice |
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