CN109275956A - A kind of additives of filter tip and preparation method thereof based on the cool taste component of the eastern purple perilla of purification - Google Patents
A kind of additives of filter tip and preparation method thereof based on the cool taste component of the eastern purple perilla of purification Download PDFInfo
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- CN109275956A CN109275956A CN201811097780.0A CN201811097780A CN109275956A CN 109275956 A CN109275956 A CN 109275956A CN 201811097780 A CN201811097780 A CN 201811097780A CN 109275956 A CN109275956 A CN 109275956A
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- cigarette
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- purple perilla
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of cigarette filter-tip additive agents, including following weight item: the eastern cool taste ingredient 20-30% of purple perilla, prune medicinal extract 1.2-1.5%, tamarind medicinal extract 1.2-1.5%, Bai Yun Shen glycosides 0.2-0.4%, essential oil of tobaccos 1.5%-2%, green tea essential oil 0.8-1.5%, glycerol 4-6%；Its surplus is triacetyl glycerine.Cooling taste, reduction cigarette smoking dry sensation and irritating purposes the invention also discloses the cool taste ingredient preparation method of the east purple perilla and for increasing cigarette smoking in cigarette filter.
Description
Technical field
The invention belongs to cigarette additive technical fields, and in particular to one kind is main to refine cool taste ingredient in eastern purple perilla
Filter tip addition of ingredient and preparation method thereof, and the cool taste ingredient of eastern purple perilla is used to deploy the purposes in cigarette filter-tip additive agent.
Background technique
Eastern purple perilla (scientific name: ElsholtziabodinieriVant.) nickname: bodinier elsholtzia herb, small camellia, Yun Songcha, herbal tea
Deng being Labiatae perennial herb, 25-30 centimetres high, pyrene oblong is about 1.1 millimeters.Contain aromatic oil in eastern purple perilla；
All herbal medicine can control affection of exogenous wind-cold, cold, fever, headache bodily pain, sore-throat, toothache caused by fire of deficiency type, indigestion, diarrhoea, mesh bitterly, suddenly
The diseases such as membranous conjunctivitis, renal shutdown and hepatitis.Its tender point can also be used when tea-drinking, there is the benefits of clearing heat and detoxicating；Fire is commonly used for Yunnan is civil
Pot shop, barbecue spread out common herbal tea and drink, it is soaked drink after can eliminate the dry sense of the heat of the throat after eating barbecue, chafing dish, promote throat and relax
Adaptive.Purple perilla is primary raw material to the east of patent of invention (CN201710197440.4) registration, prepares cigarette mouth with subcritical abstraction
The method of stick additive, but the quality quality of additive is not high, and it is not pure enough to inhale taste after adding in cigarette filter.
The present invention has invented a kind of reversed-phase resin column chromatography purification for deficiency existing for document registration method before this
The eastern cool taste compositions, method of purple perilla, sampling the method for the present invention can effectively remove bitter taste ingredient in eastern purple perilla, obtain more pure
Eastern purple perilla refine cool taste component, and be used for the cool taste ingredient of the eastern purple perilla of obtained purification that additives of filter tip is made, solve
Cigarette is sucked and dried sense and irritating problem, increases the cooling taste of cigarette smoking, improves it and aspirates comfort.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of purple with reversed-phase resin column chromatography purification east
The new method of cool taste ingredient in Soviet Union, and rely on cool taste ingredient allotment cigarette filter-tip additive agent in the eastern purple perilla of purification；The additive
It is added in cigarette filter in cigarette filter forming process, can effectively reduce cigarette dry sensation and irritation, increases cigarette and take out
The cooling taste of suction improves cigarette suction comfort.
Unless otherwise indicated, percentage of the present invention is weight percent.
The purpose of the present invention is achieved by the following technical programs.
First aspect present invention discloses a kind of cigarette filter-tip additive agent, which is characterized in that including following weight item: east
Purple perilla cool taste ingredient 20-30%, prune medicinal extract 1.2-1.5%, tamarind medicinal extract 1.2-1.5%, Bai Yun Shen glycosides 0.2-0.4%, cigarette
Careless essential oil 1.5%-2%, green tea essential oil 0.8-1.5%, glycerol 4-6%；Its surplus is triacetyl glycerine.
Preferably, the eastern cool taste ingredient of purple perilla is that the eastern cool taste ingredient of purple perilla is dissolved in triacetyl glycerine and glycerol (wherein
Triacetyl glycerine and glycerol volume ratio are the solution in 90:10).
Preferably, the eastern cool taste component extracting method of purple perilla is extracted using following extraction element and refining plant:
The extraction element includes such as lower component:
Ultrasonic extraction tank 1, upper part have feed opening 3 and pressurization mouth 4 and to be connected to extracting solution delivery pump 2, and lower part has the
One discharge port 11-1；
Filter bag 6；
Air compressor machine 5；
There are the second discharge port 11-2 in concentration tank 9, its underpart；
Condenser 10；
Solvent recovery tank 12；
The connection type of each component is as follows:
The ultrasonic extraction tank 1 is connected to by the first discharge port 11-1 with 6 upper inlet of filter bag, the ultrasonic extraction
1 top of tank is connected to the air compressor machine 5 by the pressurization mouth 4；6 lower part outlet of filter bag is connected to the concentration tank 9, described
9 top of concentration tank is connected to the entrance of the condenser 10, solvent recovery tank 12 described in 10 outlet of condenser；
The refining plant includes such as lower component:
Chromatographic column 18 is horizontally arranged, and is inside filled with resin 13, is fixed on the outside of the resin 13 by sieve plate 19；
Elution fraction collecting tank 16；
Efflux and cleaning solution collecting tank 17；
Four-way valve 14；
Triple valve 15；
The connection type of each component is as follows:
18 side sieve plate 19 of chromatographic column is connected to a valve port of the four-way valve 14, other three valves of the four-way valve 14
Mouth is respectively: a valve port a is connected to the elution fraction collecting tank 16, and b valve port b and F pump connect, and c valve port c and G are pumped and connected；Layer
Analysis 18 other side sieve plate 19 of column is connected to a valve port of the triple valve 15, other two valve port difference of the triple valve 15
Be: d valve port d is connected to the efflux and cleaning solution collecting tank 17, and e valve port e and H pump connect
The extracting method includes the following steps:
1. eastern purple perilla is crushed to 30~50 mesh powders to be added in the ultrasonic extraction tank 1, with powder weight 2~3
Times 80wt% EtOH Sonicate extract 30~50min of powder, be then forced through the filter bag 6 be obtained by filtration extracting solution enter it is dense
In contracting tank 9, filter residue with 0.5~0.8 times of powder weight of 80wt% ethanol washing and filters out cleaning solution again, merges in concentration tank 9
Extracting solution and cleaning solution, when extracting solution and cleaning solution is concentrated under reduced pressure to 40~50wt% that wherein Residual ethanol is gross mass
Obtain concentrate；
2. 1. concentrate that step is obtained is by reversed-phase resin chromatographic column 18, wherein the volume of the concentrated liquid is the dress of resin 13
Then 4~5 times for filling out volume use 1~1.5 times of resin admission space of 40~50wt% ethanol washing chromatographic column；
3. the chromatographic column 2. step is washed after is eluted with the ethyl alcohol opposite direction of 80wt%, wherein the volume of 80wt% ethyl alcohol
It is 4-5 times of resin admission space；Collect eluent and be concentrated under reduced pressure into it is solvent-free obtain described in the cool taste ingredient of eastern purple perilla.
Preferably, the resin (13) is BOSHI reversed-phase resin, the diameter of resin (13) filling: a height of 1:2, instead
It is 35~75 μm to the partial size of resin.
Second aspect of the present invention discloses the cigarette filter-tip additive agent for reducing cigarette dry sensation and irritating
Purposes.
Preferably, the reduction cigarette smoking dry sensation and irritating evaluation method use cell AQP5 expressing quantity
Evaluate the additives of filter tip reduction cigarette smoking dry sensation and irritating effect.
Illustrate with reference to the accompanying drawing the extracting method of cool taste ingredient in cigarette filter-tip additive agent of the invention and eastern purple perilla, with
And cigarette filter-tip additive agent purposes and dry sensation and irritation evaluation method step, it is specific as follows:
1, the extraction and purification of the cool taste ingredient of eastern purple perilla
A. sample extraction
Eastern purple perilla sample extraction technique uses attached device shown in FIG. 1.It takes eastern purple perilla to be crushed to 30-50 mesh powder, throws
Enter in ultrasonic extractor 1；Then 2~3 times of powder weight of 80wt% ethyl alcohol is added；30~50min of ultrasonic extraction.It has extracted
After open the first discharge port 11-1, start air compressor machine 5 to pressurizeing in ultrasonic extraction tank 1, extracting solution leads under pressure
Filter bag 6 filters；After the completion of filtering, then with 0.5~0.8 times of powder weight of 80wt% ethanol washing filter residue and filter out washing
Liquid, combined extract and cleaning solution are transferred in concentration tank 9, be concentrated under reduced pressure residual quantity of the extracting solution to concentrate to ethyl alcohol for 40~
Stop concentration when 50wt%, for column chromatography for separation.Etoh solvent enters in solvent recovery tank 12 after condenser 10 is cooling.
B. column chromatography for separation
Column chromatography for separation technique and device are as shown in Fig. 2.Gone out from the concentrate after the concentration of concentration tank 9 in Fig. 1 by second
Material mouth 11-2 discharging, conveys into being pumped in attached drawing 2 with F, enters BOSHI reversed-phase resin chromatographic column 18 by the b mouth of four-way valve 14,
Then it is flowed out by the d mouth of triple valve 15, into efflux and cleaning solution collecting tank 17.Wherein chromatographic column 18 loaded resin
Diameter: a height of 1:2, resin partial size are 35~75 μm, cross 4~5 times that column amount of solution is resin admission space.Then resin is used again
1~1.5 times of admission space of 40~50wt% ethanol washes wash chromatographic column, and cleaning solution passes through chromatographic column 18 by G pump conveying,
Cleaning solution is equally by the b mouth of four-way valve by the d mouth outflow of triple valve 15 after chromatographic column 18, into efflux and cleaning solution
In collecting tank 17.
In this process, sample solution crosses chromatographic column 18 with 40~50wt% ethyl alcohol, and with 40~50wt% ethanol washing
Chromatographic column 18 reaches efficiently separating for cool taste ingredient in eastern purple perilla and bitter component.
C. the elution and sample concentration of the cool taste ingredient of eastern purple perilla
After the completion of above-mentioned 2. column chromatography for separation step, start the H pump in Fig. 2, elutes layer with the ethyl alcohol opposite direction of 80wt%
Column is analysed, wherein the volume of 80wt% ethyl alcohol is 4-5 times of resin admission space.Eluent is by triple valve 15 in Fig. 2 during being somebody's turn to do
E mouth enter, by after chromatographic column 18 by four-way valve 14 a mouth outflow, subsequently into elution fraction collecting tank 16.
By the eluent being collected into elution fraction collecting tank 16 be concentrated under reduced pressure into it is solvent-free after obtain the east purple
Su Liang taste ingredient.Then it is dissolved into triacetyl glycerine glycerol and forms solution for standby；Wherein triacetyl glycerine with it is sweet
The volume ratio of oil is 90:10.
2, the preparation of cigarette filter-tip additive agent
Cigarette filter-tip additive agent of the present invention is made of the raw material of following mass percents: 3. Yunnan that step obtains
The eastern cool taste ingredient 20-30% of purple perilla, prune medicinal extract 1.2-1.5%, tamarind medicinal extract 1.2-1.5%, Bai Yun Shen glycosides 0.2-0.4%,
Essential oil of tobaccos 1.5%-2%, green tea essential oil 0.8-1.5%, glycerol 4-6%；Its surplus is triacetyl glycerine.Each raw material is mixed
Close the light yellow liquid uniformly obtained, as required cigarette filter-tip additive agent.The cool taste ingredient of its Middle East purple perilla is thirdly acetic acid
(triacetyl glycerine and glycerol volume ratio are added for the solution form in 90:10) for glyceride and glycerol.
Cigarette filter-tip additive agent of the present invention raw material based on the cool taste ingredient that is refined from eastern purple perilla.From eastern purple
The cool taste ingredient refined in Soviet Union not only has pure cool interest sense, but also cool taste is lasting, and retention time is long in the oral cavity, has
It obviously promotes the production of body fluid effect.
Prune medicinal extract and tamarind medicinal extract are to extract to obtain with the sour-sweet taste fruit prune in Yunnan and tamarind, common foodstuff flavouring
Agent is widely used in various beverages, carbonated drink, in candy, can assign additive pure tart flavour, sour is strong, and can neutralize part
Cigarette smoking irritation is effectively reduced in free nicotine in cigarette gas.
Bai Yun Shen glycosides is the sweetener high as sugariness made of raw material using Yunnan Special plant snow mountain Radix Glycyrrhizae, and sugariness is
600 times of sweetness of cane sugar, clean taste, pleasant impression is lasting, returns the sustainable reservation of sweet tea sense 1 hour, there is splendid shielding flue gas bitter taste
The effect of with miscellaneous gas is covered, and the cool taste components matching use of east purple perilla can increase additivated sweet tea sense, allow cigarette odor-absorbing band
There is salubrious naturally time sweet tea mouthfeel.
Green tea essential oil and essential oil of tobaccos are the extract of natural plants.Green tea essential oil has fresh and clean tea smell,
Fragrance texture is thick and heavy, and elegant fragrance is naturally, the tea perfume of cigarette smoke gracefulness can be assigned.Pure tobacco oil rich in a large amount of this perfume of tobacco at
Point, it can increase the tobacco of cigarette smoking this perfume feature, cover cigarette foreign gas, cigarette perfume is made to become more to enrich and naturally.
Glycerol has solubilization, can increase the solubility of acid, sweet ingredient in additive, and increased perfume (or spice) in formula
Gas ingredient keeps stablizing, and increases the moisture feeling of cigarette smoking.
3, additives of filter tip reduces cigarette dry sensation and irritating biological assessment
Using cell aquaporin 5 (AQP5) construct drop it is dry promote the production of body fluid model to drop additives of filter tip of the present invention into
Row evaluation.Salivary acinar cells are subjected to medical preconditioning first, it is made to simulate cell micro-environment when dry syndrome occurs,
Cell is stimulated using various concentration additives of filter tip again, the cells are fixed after stimulation, AQP5 penetrating, that FITC label is added
Antibody carries out dye marker, with high intension imaging system observation additives of filter tip treated cell AQP5 expressing quantity,
And compared with the cell controls sample handled without additives of filter tip.The result shows that: additives of filter tip of the present invention can raise carefully
Born of the same parents' AQP5 expressing quantity illustrates that it has good effect of promoting the production of body fluid, and can promote the moisture feeling of cigarette smoking, reduces irritation.
4, filter tip addition and cigarette preparation
Additives of filter tip of the invention is using triacetyl glycerine as medium.In cigarette filter forming process, filter tip is added
Agent is added to be added in cigarette filter.Cigarette for addition is cigarette product " purple cloud " or " Camellia is soft " of the Red River Hong Yun group,
It is uniformly sprayed on filter tow by the 6-8w% of filter tow weight, cigarette filter rod is made, then lead to the cigarette filter rod
It crosses conventional cigarette cigarette and cigarette is made, carry out sensory evaluating smoking, and not to the same recipe of eastern purple perilla cool taste ingredient purification
The identical cigarette of additive carries out sensory evaluating smoking as control sample.Smoking result shows: and control sample compares, filter tip of the present invention adds
Add agent to be added in the filter tip of cigarette, reduce the dry sensation and irritation of cigarette smoking, effect is clearly, moreover it is possible to assign volume
Cigarette flue gas has salubrious moisture feeling, natural sweet tea sense, and time sweet tea is lasting, pleasant impression is clean, and flue gas is softer, and fragrance is more abundant.
The result shows that the cooling taste of additives of filter tip increase cigarette smoking of the invention, the effect of improvement cigarette suction comfort are very bright
It is aobvious.
Beneficial effects of the present invention:
1, raw material, the pure nature of sweet taste based on the cool taste ingredient of purple perilla to the east of additives of filter tip of the invention.
2, have reversed-phase resin column in refining plant of the invention, using the chromatography reversed-phase resin column can refine target at
Point.BOSHI reversed-phase resin is polystyrene-divinylbenzene copolymeric material, is to separate skill based on modern HPLC liquid chromatogram
Art design, there is lesser particle and higher chromatographic separation performance, the present invention is used for plant target component for the first time
Separation and purification purification.It is compared with traditional reversed phase column chromatography material binds silica gel, there is higher adsorption capacity, stability of material
It is higher, and material cost is lower.It is also able to maintain good column and imitates for reversed resin chromatography column reusable 6000 times or more, be used for
Real cost of production is far below other column chromatography for separation techniques.
3, ultrasonic extraction device (such as Fig. 1) and automatic column chromatography device (such as Fig. 2) involved in the present invention.It is mentioned using ultrasound
Taking technique is compared with traditional Effect of Alcohol Extracting Procedureto Total, and energy consumption is reduced in extraction process, and is extracted more complete.Pass through
Automatic column chromatography technique, sample pipetting volume, washing, elution can be controlled by digital controlled valve, be able to achieve the automatic of column chromatography for separation
Change operation, production operation high degree of automation, human cost are low.
4, solvent used in the present invention is ethyl alcohol, glycerol or triacetyl glycerine etc., is common cigarette additive,
Production technology will not introduce poor solvent residual；Wherein the big etoh solvent of consumption can realize recycling and reusing, production process
Safety and environmental protection, generate consumption and it is at low cost.
5, additives of filter tip of the invention in cigarette industry using easy to accomplish.In the filter stick formation mistake of production of cigarettes
Cheng Zhong need to add triacetyl glycerine as the plasticizer in cigarette filter molding, and additive amount is the 6- of filter stick tow weight
8%.Additives of filter tip of the invention is targetedly sweet using three acetic acid the problem of the design phase just considering industrial application
Grease additive preparation；The principal component of gained additives of filter tip is that (95wt% for accounting for additives ratio is left for triacetyl glycerine
It is right), in this way, plasticizer triacetyl glycerine can be substituted with additive of the present invention in cigarette filter forming process, filter stick at
Type process needs to increase additional process, and industrial application is very easy to realize.
6, the present invention is except in addition to raw material based on eastern purple perilla, also using a variety of natural plant extracts and monomer chosen
Fragrance deploys additive, by the synergistic effect of they and the cool taste ingredient of eastern purple perilla, enriches the perfume (or spice) of additives of filter tip
Gas is rich, promotes and improve the effect of cigarette suction comfort.
7, the dry effect of promoting the production of body fluid of drop of additive of the present invention is evaluated in the present invention using up-regulation cell AQP5 expressing quantity
Fruit and traditional artificial sense are evaluated to form supplement, improve can additives of filter tip effect assessment objectivity.
Detailed description of the invention
Fig. 1 is eastern purple perilla sample extraction process device figure.
Fig. 2 is the cool taste ingredient process for refining device figure of eastern purple perilla.
Appended drawing reference are as follows: 1, ultrasonic extraction tank；2, liquid pump is extracted in conveying；3, feed opening；4, pressurize mouth；5, air compressor machine；6,
Filter bag；7, enamel interface；8, valve；9, concentration tank；10, condenser；11-1, the first discharge port；11-2, the second discharge port；12,
Alcohol recovering device；13, vacuum tube；14, four-way valve；15, triple valve；16 elution fraction collecting tanks；17, efflux and cleaning solution
Collecting tank；18, chromatographic column；19, sieve plate；F, F is pumped；G, G is pumped；H, H is pumped；A, four-way valve a mouthfuls；B, four-way valve b mouthfuls；C, four-way valve c
Mouthful；D, triple valve d mouthfuls；E, triple valve e mouthfuls.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right below in conjunction with drawings and examples
The present invention is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.If not raw material employed in embodiment and equipment are refered in particular to, it is commercially available or this field
Commonly, the method in embodiment is unless otherwise instructed the conventional method of this field.
Embodiment 1: the extraction and purification of the eastern cool taste ingredient of purple perilla
A, sample extraction
As shown in Fig. 1, it takes eastern purple perilla to be crushed to 40 mesh powders to put into ultrasonic extraction tank 1 by feed opening 3；So
2 times of powder weight of 80wt% ethyl alcohol is added afterwards；Ultrasonic extraction 30min opens discharge port 11-1 after the completion, starts air compressor machine 5
To pressurizeing in ultrasonic extraction tank 1, extracting solution passes through filter bag 6 under pressure and filters；After the completion of filtering, then with powder weight
The 80wt% ethanol solution washing filter residue of 0.5 times of amount simultaneously filters out cleaning solution, and combined extract and cleaning solution are transferred in concentration tank 9.
When reduced pressure extracting solution and cleaning solution to Residual ethanol are 50wt%, for column chromatography for separation.Etoh solvent is through condenser
Enter in solvent recovery tank 12 after 10 coolings.
B, the separation of cool taste ingredient
As shown in Fig. 2, the concentrate flowed out from the discharge port 11-2 of concentration tank 9 is anti-by BOSHI by F pump conveying in Fig. 2
Phase resin chromatography column 18,18 loaded resin of chromatographic column, 13 particle, the diameter of resin 13: a height of 1:2, resin partial size are 35 μm, mistake
Column amount of solution is 4 times of resin admission space.In this process, sample solution is by b mouthfuls of four-way valve in Fig. 2 into passing through chromatography
By d mouthfuls of triple valve outflows in Fig. 2 after column 18；It has crossed after column and has used 1 times of resin admission space of 25wt% ethanol washing chromatographic column,
Cleaning solution by G pump conveying in Fig. 2 by chromatographic column 18, cleaning solution by four-way valve c mouthfuls in Fig. 2 into, by after chromatographic column 18 by scheming
Triple valve d flows out in 2.In this process, sample solution crosses chromatographic column 18 with 50wt% ethanol medium, and with 50wt% ethyl alcohol
Wash chromatographic column 18.Efflux and cleaning solution enter in efflux and cleaning solution collecting tank 17.
C, the elution and concentration of cool taste ingredient
After the completion of washing in above-mentioned steps, start the H pump in Fig. 2, with the ethyl alcohol opposite direction elution chromatography column of 80wt%
18, effluent volume is 4 times of 13 volume of chromatographic column filling resin.Ethyl alcohol of 80wt% is by triple valve e mouthfuls in Fig. 2 during this
Into by entering elution fraction collecting tank 16 by four a mouthfuls of valve outflows after chromatographic column, by elution fraction collecting tank after the completion of elution
Eluent in 16 is concentrated under reduced pressure to dry, solvent-free to get taste ingredient cool into eastern purple perilla, and it is sweet to be then dissolved in three acetic acid
Grease and glycerol in the mixed solvent (triacetyl glycerine and glycerol volume ratio be 90:10).
Embodiment 2: the extraction and purification of the eastern cool taste ingredient of purple perilla
A, sample extraction
As shown in Fig. 1, eastern purple perilla is taken to be crushed in 45 mesh powders investment ultrasonic extraction tank；Then to ultrasonic extraction tank
The middle 80wt% ethyl alcohol for being added 3 times of powder weight；Ultrasonic extraction 50min.Discharge port is opened after having extracted, starting air compressor machine is to super
It pressurizes in sound extractor, extracting solution passes through sock filtration under pressure；After the completion of filtering, then with example weight 0.8
80wt% ethanol washing filter residue again simultaneously filters out cleaning solution, and combined extract and cleaning solution are transferred in concentration tank 9.Reduced pressure mentions
Taking liquid and cleaning solution to Residual ethanol is 40wt%, for column chromatography for separation.
B, the separation of cool taste ingredient
As shown in Fig. 2, the concentrate flowed out from the discharge port 11-2 of concentration tank 9 is anti-by BOSHI by F pump conveying in Fig. 2
Phase resin chromatography column (diameter of chromatographic column filling resin filling: a height of 1:2, reversed resin partial size are 75 μm), crosses column amount of solution
It is 5 times of resin admission space.In this process, sample solution by b mouthfuls of four-way valve in Fig. 2 into, by after chromatographic column 18 by
D mouthfuls of triple valve outflows in Fig. 2；It has crossed after column and has used 1.5 times of resin admission space of 40wt% ethanol washing chromatographic column, cleaning solution
By G pump conveying in Fig. 2 by chromatographic column 18, cleaning solution by four-way valve c mouthfuls in Fig. 2 into, by after chromatographic column 18 by threeway in Fig. 2
Valve d outflow.In this process, sample solution crosses chromatographic column 18 with 40wt% ethanol medium, and is chromatographed with 40wt% ethanol washing
Column 18.
C, the elution and concentration of cool taste ingredient
After the completion of washing in above-mentioned steps, start the H pump in Fig. 2, with the ethyl alcohol opposite direction elution chromatography column of 80wt%
18, effluent volume is 5 times of chromatographic column filling resin volume.Ethyl alcohol of 80wt% is by triple valve e mouthfuls in Fig. 2 during this
Into, by after chromatographic column by four a mouthfuls of valve outflow enter elution fraction collecting tank 16, elution fraction is collected after the completion of elution
Eluent in tank 16 is concentrated under reduced pressure to dry, solvent-free to get taste ingredient cool into eastern purple perilla, is then dissolved in three acetic acid
Glyceride and glycerol in the mixed solvent (triacetyl glycerine and glycerol volume ratio be 90:10).
Embodiment 3: the extraction and purification of the eastern cool taste ingredient of purple perilla
A, sample extraction
As shown in Fig. 1, eastern purple perilla is taken to be crushed in 30 mesh powders investment ultrasonic extraction tank；Then to ultrasonic extraction tank
The middle 80wt% ethyl alcohol for being added 2.5 times of powder weight；Ultrasonic extraction 40min.Discharge port is opened after having extracted, and starts air compressor machine pair
It pressurizes in ultrasonic extraction tank, extracting solution passes through sock filtration under pressure；After the completion of filtering, then use example weight
0.6 times of 80wt% ethanol washing filter residue simultaneously filters out cleaning solution, and combined extract and cleaning solution are transferred in concentration tank 9.It depressurizes dense
Contracting extracting solution and cleaning solution to Residual ethanol are 45wt%, for column chromatography for separation.
B, the separation of cool taste ingredient
As shown in Fig. 2, the concentrate flowed out from the discharge port 11-2 of concentration tank 9 is anti-by BOSHI by F pump conveying in Fig. 2
Phase resin chromatography column (diameter of chromatographic column filling resin filling: a height of 1:2, reversed resin partial size are 50 μm), crosses column amount of solution
It is 4 times of resin admission space.In this process, sample solution by b mouthfuls of four-way valve in Fig. 2 into, by after chromatographic column 18 by
D mouthfuls of triple valve outflows in Fig. 2；Crossed after column and used 1 times of resin admission space of 45wt% ethanol washing chromatographic column, cleaning solution by
The conveying of G pump is by chromatographic column 18 in Fig. 2, cleaning solution by four-way valve c mouthfuls in Fig. 2 into, by after chromatographic column 18 by triple valve in Fig. 2
D outflow.In this process, sample solution crosses chromatographic column 18 with 45wt% ethanol medium, and with 45wt% ethanol washing chromatographic column
18。
C, the elution and concentration of cool taste ingredient
After the completion of washing in above-mentioned steps, start the H pump in Fig. 2, with the ethyl alcohol opposite direction elution chromatography column of 80wt%
18, effluent volume is 5 times of chromatographic column filling resin volume.Ethyl alcohol of 80wt% is by triple valve e mouthfuls in Fig. 2 during this
Into, by after chromatographic column by four a mouthfuls of valve outflow enter elution fraction collecting tank 16, elution fraction is collected after the completion of elution
Eluent in tank 16 is concentrated under reduced pressure to dry, solvent-free to get taste ingredient cool into eastern purple perilla, is then dissolved in three acetic acid
Glyceride and glycerol in the mixed solvent (triacetyl glycerine and glycerol volume ratio be 90:10).
Embodiment 4: the preparation of additives of filter tip
Cigarette filter-tip additive agent of the present invention is made of the raw material of following mass percents: the Yunnan that embodiment 1 obtains
The eastern cool taste ingredient of purple perilla is 20%, and prune medicinal extract is 1.2%, and tamarind medicinal extract is 1.2%, Bai Yun Shen glycosides 0.2%, essential oil of tobaccos
1.5%, green tea essential oil 0.8%, glycerol 4%, surplus is triacetyl glycerine.By each raw material be uniformly mixed obtain it is light yellow
Liquid, as required cigarette filter-tip additive agent.
Embodiment 5: the preparation of additives of filter tip
Cigarette filter-tip additive agent of the present invention is made of the raw material of following mass percents: the east that embodiment 2 obtains is purple
Su Liang taste ingredient 30%, prune medicinal extract 1.3%, tamarind medicinal extract 1.5%, Bai Yun Shen glycosides 0.4%, essential oil of tobaccos 1.8%, green tea essence
Oil 1.2%, glycerol 5%；Its surplus is triacetyl glycerine.Each raw material is uniformly mixed to obtained light yellow liquid, as institute
The cigarette filter-tip additive agent needed.
Embodiment 6: the preparation of additives of filter tip
Cigarette filter-tip additive agent of the present invention is made of the raw material of following mass percents: the Yunnan that embodiment 3 obtains
The eastern cool taste ingredient of purple perilla is 25%, and prune medicinal extract is 1.5%, and tamarind medicinal extract is 1.2%, and Bai Yun Shen glycosides is 0.4%, essential oil of tobaccos
1.8%, green tea essential oil 1.2%, glycerol 6%；Its surplus is triacetyl glycerine.By each raw material be uniformly mixed obtain it is light yellow
Liquid, as required cigarette filter-tip additive agent.
Embodiment 7: the biological assessment of additives of filter tip
Any additives of filter tip of Example 4-6 preparation carries out reducing the test of cigarette irritation biological assessment, test
Steps are as follows:
The dry model that promotes the production of body fluid of the drop constructed using cell aquaporin 5 (AQP5) carries out additives of filter tip of the present invention
Evaluation.Salivary acinar cells are subjected to medical preconditioning, so that it is simulated cell micro-environment when dry syndrome occurs, then use
Various concentration additives of filter tip stimulate cell, the cells are fixed after stimulation, it is penetrating, be added FITC label AQP5 antibody into
Row dye marker, with high intension imaging system observation additives of filter tip treated cell AQP5 expressing quantity, and with not
The cell controls sample handled through additives of filter tip compares.The result shows that: additives of filter tip of the present invention can raise cell AQP5
Expressing quantity illustrates that it has good effect of promoting the production of body fluid, and can promote the moisture feeling of cigarette smoking, reduces dry sensation and irritation.
Embodiment 8: application of the additives of filter tip in cigarette
Additives of filter tip in Example 4 carries out the additive effect experiment of cigarette filter, and test situation is as follows:
For the cigarette " purple cloud " that addition cigarette is the Red River Hong Yun group, by additive of the present invention by filter tow weight
6% is uniformly sprayed on filter tow filter stick is made, and cigarette then is made in the filter stick cigarette, carries out sensory evaluating smoking, and with
Sensory evaluating smoking is not carried out as control sample to the identical cigarette of the additive of the same recipe of eastern purple perilla cool taste ingredient purification.It smokes panel test
The result shows that: it compares with control sample, the dry sensation and irritant effects of additives of filter tip reduction cigarette smoking of the invention are non-
Chang Mingxian, moreover it is possible to cooling taste, the cigarette smoking pleasant impression for increasing cigarette smoking are cleaner, and flue gas is softer, and fragrance is more abundant,
The effect that cigarette suction comfort improves is clearly.
Embodiment 9: application of the additives of filter tip in cigarette
Additives of filter tip in Example 6 carries out the additive effect experiment of cigarette filter, and test situation is as follows:
For the cigarette " Camellia is soft " that addition cigarette is the Red River Hong Yun group, additive of the present invention is pressed into filter tow weight
The 6% of amount is uniformly sprayed on filter tow and filter stick is made, and cigarette then is made by cigarette in the filter stick, carries out sense organ and comments
It inhales, and sense organ is carried out as control sample using the identical cigarette of the additive not to the same recipe of eastern purple perilla cool taste ingredient purification and is commented
It inhales.Smoking result shows: comparing with control sample, additives of filter tip of the invention reduces the dry sensation and irritation of cigarette smoking
Effect clearly, increases the cooling taste effect of cigarette smoking, improves the sweet tea sense of cigarette smoking, keeps cigarette smoking pleasant impression more dry
Only, flue gas is softer, and fragrance is more abundant, and the effect that cigarette suction comfort improves is obvious.
Those skilled in the art is it should be appreciated that the present invention is not limited to the above embodiments, above-described embodiment and explanation
It is merely illustrated the principles of the invention described in book, without departing from the spirit and scope of the present invention, the present invention also has
Various changes and modifications, these changes and improvements are both fallen in the claimed scope of the invention.
Claims (6)
1. a kind of cigarette filter-tip additive agent, which is characterized in that including following weight item: the eastern cool taste ingredient 20-30% of purple perilla, west
Plum medicinal extract 1.2-1.5%, tamarind medicinal extract 1.2-1.5%, Bai Yun Shen glycosides 0.2-0.4%, essential oil of tobaccos 1.5%-2%, green tea essence
Oily 0.8-1.5%, glycerol 4-6%；Its surplus is triacetyl glycerine.
2. according to cigarette filter-tip additive agent according to claim 1, which is characterized in that the east cool taste ingredient of purple perilla is east
The cool taste ingredient of purple perilla is dissolved in molten in triacetyl glycerine and glycerol (wherein triacetyl glycerine and glycerol volume ratio are 90:10)
Liquid.
3. cigarette filter-tip additive agent according to claim 1, which is characterized in that the cool taste component extracting method of the east purple perilla
It is extracted using following extraction element and refining plant:
The extraction element includes such as lower component:
Ultrasonic extraction tank (1), upper part have feed opening (3) and pressurization mouth (4) and are connected to extracting solution delivery pump (2), lower part
There is the first discharge port (11-1)；
Filter bag (6)；
Air compressor machine (5)；
Concentration tank (9), its underpart have the second discharge port (11-2)；
Condenser (10)；
Solvent recovery tank (12)；
The connection type of each component is as follows:
The ultrasonic extraction tank (1) is connected to by the first discharge port (11-1) with the filter bag (6) upper inlet, and the ultrasound mentions
Tank (1) top is taken to be connected to the air compressor machine (5) by the pressurization mouth (4)；Filter bag (6) lower part outlet and the concentration tank
(9) it is connected to, the entrance of concentration tank (9) the top connection condenser (10), described in condenser (10) outlet
Solvent recovery tank (12)；
The refining plant includes such as lower component:
Chromatographic column (18) is horizontally arranged, is inside filled with resin (13), solid by sieve plate (19) on the outside of the resin (13)
It is fixed；
Elution fraction collecting tank (16)；
Efflux and cleaning solution collecting tank (17)；
Four-way valve (14)；
Triple valve (15)；
The connection type of each component is as follows:
Chromatographic column (18) side sieve plate (19) is connected to a valve port of the four-way valve (14), the four-way valve (14) other three
A valve port is respectively: a valve port (a) is connected to the elution fraction collecting tank (16), and b valve port (b) and F pump connect, c valve port (c)
It pumps and connects with G；Chromatographic column (18) other side sieve plate (19) is connected to a valve port of the triple valve (15), the triple valve (15)
Other two valve ports be respectively: d valve port (d) is connected to the efflux and cleaning solution collecting tank (17), and e valve port (e) and H are pumped
Connection
The extracting method includes the following steps:
1. eastern purple perilla is crushed to 30~50 mesh powders to be added in the ultrasonic extraction tank (1), with 2~3 times of powder weight
80wt% EtOH Sonicate extract 30~50min of powder, be then forced through the filter bag (6) be obtained by filtration extracting solution enter it is dense
In contracting tank (9), filter residue with 0.5~0.8 times of powder weight of 80wt% ethanol washing and filters out cleaning solution again, merges concentration tank
(9) extracting solution and cleaning solution in, be concentrated under reduced pressure extracting solution and cleaning solution to 40 that wherein Residual ethanol is gross mass~
Concentrate is obtained when 50wt%；
2. 1. concentrate that step is obtained is by reversed-phase resin chromatographic column (18), wherein the volume of the concentrated liquid is resin (13) filling
Then 4~5 times of volume use 1~1.5 times of resin admission space of 40~50wt% ethanol washing chromatographic column；
3. the chromatographic column 2. step is washed after is eluted with the ethyl alcohol opposite direction of 80wt%, wherein the volume of 80wt% ethyl alcohol is tree
4-5 times of rouge admission space；Collect eluent and be concentrated under reduced pressure into it is solvent-free obtain described in the cool taste ingredient of eastern purple perilla.
4. cigarette filter-tip additive agent according to claim 3, which is characterized in that the resin (13) is BOSHI reverse phase tree
Rouge, the diameter of resin (13) filling: a height of 1:2, the partial size of reversed resin are 35~75 μm.
5. cigarette filter-tip additive agent according to claim 1 to 4 is for reducing cigarette dry sensation and irritating use
On the way.
6. purposes according to claim 5, which is characterized in that the reduction cigarette smoking dry sensation and irritating evaluation
Method using cell AQP5 expressing quantity evaluate the additives of filter tip reduction cigarette smoking dry sensation and irritating effect
Fruit.
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| CN201811097780.0A CN109275956B (en) | 2018-09-20 | 2018-09-20 | Filter tip additive mainly containing refined perilla frutescens cool taste component and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109998165A (en) * | 2019-04-03 | 2019-07-12 | 红云红河烟草(集团)有限责任公司 | Cigarette filter stick plasticizer, preparation method thereof and cigarette filter stick |
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