CN109288125A - It is a kind of to refine the additives of filter tip and preparation method thereof based on snow mountain Radix Glycyrrhizae sweet ingredient - Google Patents
It is a kind of to refine the additives of filter tip and preparation method thereof based on snow mountain Radix Glycyrrhizae sweet ingredient Download PDFInfo
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- CN109288125A CN109288125A CN201811097929.5A CN201811097929A CN109288125A CN 109288125 A CN109288125 A CN 109288125A CN 201811097929 A CN201811097929 A CN 201811097929A CN 109288125 A CN109288125 A CN 109288125A
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- radix glycyrrhizae
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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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Abstract
The invention discloses a kind of cigarette filter-tip additive agents, including following weight item: snow mountain Radix Glycyrrhizae sweet ingredient 20-30%, acid Chinese quince medicinal extract 1.2-1.5%, green plum medicinal extract 1.2-1.5%, neohesperidin dihydrochalcone 0.2-0.4%, plateau Rosa Damascana 0.05%-0.1%, essential oil of tobaccos 1.5%-2%, eastern Fructus Perillae quintessence oil 0.8-1.5%, glycerol 4-6%；Its surplus is triacetyl glycerine.The invention also discloses the snow mountain Radix Glycyrrhizae sweet ingredient preparation method and for reducing cigarette smoking dry sensation and irritating purposes in cigarette filter.
Description
Technical field
The invention belongs to cigarette additive technical fields, and in particular to one kind is main to refine snow mountain Radix Glycyrrhizae sweet ingredient
Filter tip addition of ingredient and preparation method thereof, and snow mountain Radix Glycyrrhizae sweet ingredient is used to deploy the use in cigarette filter-tip additive agent
On the way.
Background technique
Snow mountain Radix Glycyrrhizae (Phlomisbetonicoides Diels) is Labiatae (Lamiaceae) Paraphlomis, the alias vacation Qin
Macrophylla, Bai Yun Shen, white American ginseng, white radix scrophulariae, native Radix Glycyrrhizae, white radix scrophulariae, pungent ginseng etc..Be distributed in the Yunnan Province northwestward, South-west Sichuan and
Eastern Tibet.This kind of root can be used as medicine, and can control indigestion, abdominal distension, have sore throat, traumatic consumptive injury, pneumonia, and solve in various drugs
Poison.The sugariness of main sweet substance Bai Yun Shen glucoside is 600 times of sucrose in snow mountain Radix Glycyrrhizae, and sweet taste is pure, and sweet taste can be protected
1h or so is held, oral cavity pleasant impression is very comfortable, and the plant is in Lijiang, yunnan, Shangri-la, Nujiang and Eastern Tibet, Si Chuanxi
Portion's equal distribution is extensive.Document [food industry, 2016,37 (12): 142-145) it reports and progress is joined to Bai Yun Shen glucoside using complex enzyme
Enzymolysis liquid is concentrated enzymolysis and extraction, and extra amino acid carries out Maillard reaction and prepares tobacco aromaticss.The subcritical extraction of document registration
It takes (CN201710198020.8) or heating and refluxing extraction (CN201610915435.8) to prepare snow mountain Radix Glycyrrhizae extract and is used as volume
Cigarette filter additive can effectively increase the sweet sense of cigarette smoke, improve the comfort of cigarette smoking.But sweet tea is removed in snow mountain Radix Glycyrrhizae
Outside taste ingredient, also contain bitter principle (Chem.Pharm.Bull., 1983,31 (2): 780-783), if cannot be to bitter taste
Ingredient is separated, and the quality quality of additive is not high, keeps the suction taste of cigarette smoke not pure enough 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
Snow mountain Radix Glycyrrhizae sweet ingredient method, sampling the method for the present invention can effectively remove bitter principle, it is sweet to obtain more pure snow mountain
Grass purification sweet taste component, and be used for the snow mountain Radix Glycyrrhizae sweet ingredient of obtained purification that additives of filter tip is made, solve cigarette
Be sucked and dried sense and irritating problem, improve its aspirate 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 reversed-phase resin column chromatography purification snow mountain
The new method of sweet ingredient in Radix Glycyrrhizae, and rely on sweet ingredient allotment cigarette filter-tip additive agent in the snow mountain Radix Glycyrrhizae of purification；This adds
Add agent to be added in cigarette filter in cigarette filter forming process, can effectively reduce cigarette dry sensation and irritation, improves volume
Cigarette aspirates 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: snow
Mountain Radix Glycyrrhizae sweet ingredient 20-30%, acid Chinese quince medicinal extract 1.2-1.5%, green plum medicinal extract 1.2-1.5%, neohesperidin dihydro Cha Er
Ketone 0.2-0.4%, plateau Rosa Damascana 0.05%~0.1%, essential oil of tobaccos 1.5%~2%, eastern Fructus Perillae quintessence oil 0.8-1.5%,
Glycerol 4~6%；Its surplus is triacetyl glycerine.
Preferably, the snow mountain Radix Glycyrrhizae sweet ingredient is that snow mountain Radix Glycyrrhizae sweet ingredient is dissolved in triacetyl glycerine and glycerol
Solution in (wherein triacetyl glycerine and glycerol volume ratio are 90:10).
Preferably, the snow mountain Radix Glycyrrhizae sweet ingredient extracting method is mentioned using following extraction element and refining plant
It takes:
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. snow mountain Radix Glycyrrhizae is crushed to 30~50 mesh powders to be added in the ultrasonic extraction tank 1, with powder weight 2~
3 times of 80wt% EtOH Sonicate extracts 30~50min of powder, is then forced through the filter bag 6 and extracting solution entrance is obtained by filtration
In concentration 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
In extracting solution and cleaning solution, 50~60wt% that extracting solution and cleaning solution are gross mass to wherein Residual ethanol is concentrated under reduced pressure
When 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 50~60wt% ethanol washing chromatographic column of 1~1.5 times of 13 admission space of resin；
3. the chromatographic column 18 2. step is washed after is eluted with the ethyl alcohol opposite direction of 80wt%, wherein the body of 80wt% ethyl alcohol
Product is 4-5 times of resin admission space；Collect eluent and be concentrated under reduced pressure into it is solvent-free obtain described in snow mountain Radix Glycyrrhizae sweet taste
Ingredient.
Preferably, the resin 13 is BOSHI reversed-phase resin, the diameter that the resin 13 loads: a height of 1:2, reversed tree
The partial size of rouge is 35~75 μm.
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 sweet ingredient in cigarette filter-tip additive agent and snow mountain Radix Glycyrrhizae of the invention,
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 snow mountain Radix Glycyrrhizae sweet ingredient
A. sample extraction
Snow mountain Radix Glycyrrhizae sample extraction technique uses attached device shown in FIG. 1.Snow mountain Radix Glycyrrhizae is taken to be crushed to the powder of 30-50 mesh
End is put into ultrasonic extraction tank 1；Then 2~3 times of powder weight of 80wt% ethyl alcohol is added；30~50min of ultrasonic extraction.It mentions
The first discharge port 11-1 is opened after taking, to pressurizeing in ultrasonic extraction tank 1, extracting solution acts on starting air compressor machine 5 in pressure
It is filtered by filter bag 6 down；After the completion of filtering, then with 0.5~0.8 times of powder weight of 80wt% ethanol washing filter residue and filter out
Cleaning solution, combined extract and cleaning solution are transferred in concentration tank 9, and residual quantity of the extracting solution to concentrate to ethyl alcohol is concentrated under reduced pressure and is
Stop concentration when 50~60wt%, for column chromatography for separation.Etoh solvent enters solvent recovery tank 12 after condenser 10 is cooling
In.
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 25~30wt% 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 50~60wt% ethyl alcohol, and with 50~60wt% ethanol washing
Chromatographic column 18 reaches efficiently separating for sweet ingredient in snow mountain Radix Glycyrrhizae and bitter component.
C. the elution and sample concentration of snow mountain Radix Glycyrrhizae sweet ingredient
After the completion of above-mentioned column chromatography for separation step, start the H pump in Fig. 2, with the ethyl alcohol opposite direction elution chromatography of 65wt%
Column, wherein the volume of 65wt% ethyl alcohol is 4-5 times of resin admission space.During this eluent by triple valve 15 in Fig. 2 e
Mouth enters, by being flowed out after chromatographic column 18 by a mouth of four-way valve 14, 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 described in snow mountain
Radix Glycyrrhizae sweet ingredient.Then it is dissolved into triacetyl glycerine glycerol and forms solution for standby；Wherein triacetyl glycerine with
The volume ratio of glycerol 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: the Yunnan snow that step C is obtained
Mountain Radix Glycyrrhizae sweet ingredient 20-30%, acid Chinese quince medicinal extract 1.2-1.5%, green plum medicinal extract 1.2-1.5%, neohesperidin dihydro Cha Er
Ketone 0.2-0.4%, plateau Rosa Damascana 0.05%-0.1%, essential oil of tobaccos 1.5%-2%, eastern Fructus Perillae quintessence oil 0.8-1.5% are sweet
Oily 4-6%；Its surplus is triacetyl glycerine.Each raw material is uniformly mixed to obtained light yellow liquid, as required cigarette
Additives of filter tip.Wherein snow mountain Radix Glycyrrhizae sweet ingredient is with the solution in its triacetyl glycerine and glycerol (volume ratio 90:10)
Form is added.
Cigarette filter-tip additive agent of the present invention raw material based on the sweet ingredient that is refined from snow mountain Radix Glycyrrhizae.From snow
The sweet ingredient refined in the Radix Glycyrrhizae of mountain not only has pure time sweet tea mouthfeel, and there are also strong to return sweet tea sense, and 1h can be kept by returning sweet taste
Left and right can assign time sweet tea pleasant impression as snug as a bug in a rug to oral cavity.
Acid Chinese quince medicinal extract and green plum medicinal extract are to extract to obtain with the sour-sweet taste fruit acid Chinese quince in Yunnan and green plum, common food
Flavoring agent is widely used in various beverages, carbonated drink, candy, can assign additive pure tart flavour, and sour is strong, and can neutralize portion
Cigarette smoking irritation is effectively reduced in free nicotine in bundling flue gas.
Neohesperidin dihydrochalcone is that citrus peel is the high sweetener of sugariness made of raw material, and sugariness is sugarcane
1500-1800 times of sugared sugariness, clean taste, pleasant impression is lasting, there is the effect of splendid shielding bitter taste and cover miscellaneous gas, and snow
The sweet ingredient of mountain Radix Glycyrrhizae, which is used cooperatively, can increase additivated sweet tea sense, make sweet taste richer and salubrious nature.
Plateau Rosa Damascana, eastern Fructus Perillae quintessence oil and essential oil of tobaccos are natural plant extracts.Plateau Rosa Damascana has
The distinctive faint scent of strong rose and fragrant and sweet, fragrance texture is thick and heavy, and elegant fragrance is naturally, can assign cigarette smoke graceful clear
It is fragrant and sweet.Eastern Fructus Perillae quintessence oil fragrance is fresh and sweet, and with simple and elegant green grass perfume sweet gas taste and cool taste, the stimulation of cigarette smoke can be effectively reduced
Property, enrich the fragrance of flue gas.Pure tobacco oil is rich in a large amount of this perfume of tobacco ingredients, can increase the tobacco of cigarette smoking this perfume feature,
Cigarette foreign gas is covered, cigarette perfume is made to become more to enrich and natural.
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 snow mountain Radix Glycyrrhizae sweet ingredient purification
Additive identical cigarette as control sample carry out sensory evaluating smoking.Smoking result shows: and control sample compares, filter tip of the present invention
Additive is added in the filter tip of cigarette, reduces the dry sensation and irritation of cigarette smoking, effect is clearly, moreover it is possible to assign
Cigarette smoke 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 richer
It is rich.The result shows that additives of filter tip of the invention improves the effect of cigarette suction comfort clearly.
Beneficial effects of the present invention:
1, the additives of filter tip of the invention raw material based on snow mountain Radix Glycyrrhizae sweet ingredient, the pure nature of sweet taste.
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 snow mountain Radix Glycyrrhizae, also using a variety of natural plant extracts and list chosen
Body note material deploys additive, by the synergistic effect of they and snow mountain Radix Glycyrrhizae sweet ingredient, enriches additives of filter tip
Fragrance it is rich, promote 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 snow mountain Radix Glycyrrhizae sample extraction process device figure.
Fig. 2 is snow mountain Radix Glycyrrhizae sweet ingredient process for refining device figure.
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 snow mountain Radix Glycyrrhizae sweet ingredient
A, sample extraction
As shown in Fig. 1, snow mountain Radix Glycyrrhizae is taken to be crushed in 40 mesh powders investment ultrasonic extraction tank；Then powder weight is added
The 80wt% ethyl alcohol of 2 times of amount；Ultrasonic extraction 30min opens discharge port 11-1 after the completion, starts air compressor machine to ultrasonic extraction tank 1
It inside pressurizes, extracting solution passes through filter bag 6 under pressure and filters；After the completion of filtering, then with 0.5 times of powder weight
80wt% ethanol solution washing filter residue simultaneously filters out cleaning solution, and combined extract and cleaning solution are transferred in concentration tank 9.Reduced pressure mentions
Take liquid and cleaning solution to Residual ethanol be 50wt% when, for column chromatography for separation.
B, the separation of sweet 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 35 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 50wt% 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 50wt% ethanol medium, and with 50wt% ethanol washing chromatographic column
18。
C, the elution and concentration of sweet 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 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 the sweet ingredient into snow mountain Radix Glycyrrhizae, is then dissolved in three vinegar
Acid glyceride and glycerol in the mixed solvent (triacetyl glycerine and glycerol volume ratio be 90:10).
Embodiment 2: the extraction and purification of snow mountain Radix Glycyrrhizae sweet ingredient
A, sample extraction
As shown in Fig. 1, it takes snow mountain Radix Glycyrrhizae to be crushed to 45 mesh powders to put into ultrasonic extraction tank 1 by feed opening 3, so
Ultrasonic extraction 50min after 3 times of snow mountain Radix Glycyrrhizae powder weight of 80wt% ethyl alcohol is added in backward ultrasonic extraction tank 1.After having extracted
Discharge port 11-1 is opened, starts air compressor machine 5 to pressurizeing in ultrasonic extraction tank 1, extracting solution passes through filter bag 6 under pressure
Filtering；After the completion of filtering, then with 0.8 times of example weight of 80wt% ethanol washing filter residue and cleaning solution is filtered out, combined extract
It is transferred in concentration tank 9 with cleaning solution.When reduced pressure extracting solution and cleaning solution to Residual ethanol are 60wt%, for column chromatography point
From with.Etoh solvent enters in solvent recovery tank 12 after condenser 10 is cooling.
B, the separation of sweet 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 13 of chromatographic column, the diameter that resin 13 loads: a height of 1:2,13 partial size of resin are 75 μm,
Cross 5 times that 18 amount of solution of chromatographic column is resin admission space.In this process, sample solution by b mouthfuls of four-way valve in Fig. 2 into,
By being flowed out after chromatographic column 18 by d mouthfuls of triple valve in Fig. 2；It has crossed after column and has used 1.5 times of resin admission space of 60wt% ethyl alcohol
Wash chromatographic column, cleaning solution is by G pump conveying in Fig. 2 by chromatographic column 18, and cleaning solution is by four-way valve c mouthfuls in Fig. 2 into passing through chromatography
It is flowed out after column 18 by triple valve d in Fig. 2.In this process, sample solution crosses chromatographic column 18 with 60wt% ethanol medium, is used in combination
60wt% ethanol washing chromatographic column 18.Efflux and cleaning solution enter in efflux and cleaning solution collecting tank 17.
C, the elution and concentration of sweet 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 18 loaded resin of chromatographic column, 13 volume.Ethyl alcohol of 80wt% is by triple valve e in Fig. 2 during this
Mouthful into, by after chromatographic column 18 by four a mouthful of valve outflows into elution fraction collecting tank 16, elution fraction is received after the completion of elution
Collect the eluent in tank 16 to be concentrated under reduced pressure to dry, it is solvent-free to get the sweet ingredient into snow mountain Radix Glycyrrhizae, then it is dissolved in three
Acetoglyceride and glycerol in the mixed solvent (triacetyl glycerine and glycerol volume ratio be 90:10).
Embodiment 3: the extraction and purification of snow mountain Radix Glycyrrhizae sweet ingredient
A, sample extraction
As shown in Fig. 1, snow mountain Radix Glycyrrhizae is taken to be crushed in 30 mesh powders investment ultrasonic extraction tank；Then to ultrasonic extraction
2.5 times of powder weight of 80wt% ethyl alcohol is added in tank；Ultrasonic extraction 40min.Discharge port is opened after having extracted, and starts air compressor machine
To pressurizeing 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 55wt%, for column chromatography for separation.
B, the separation of sweet 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 55wt% 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 55wt% ethanol medium, and with 55wt% ethanol washing chromatographic column
18。
C, the elution and concentration of sweet 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 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 the sweet ingredient into snow mountain Radix Glycyrrhizae, 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 snow mountain that embodiment 1 obtains
Radix Glycyrrhizae sweet ingredient 20%, acid Chinese quince medicinal extract 1.2%, green plum medicinal extract 1.2%, neohesperidin dihydrochalcone 0.2%, plateau rose
Rare essential oil 0.05%%, essential oil of tobaccos 1.5%%, eastern Fructus Perillae quintessence oil 0.8%, glycerol 4%；Its surplus is triacetyl glycerine.
Each raw material is uniformly mixed to obtained 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 snow mountain that embodiment 2 obtains
Radix Glycyrrhizae refines sweet ingredient 30%, acid Chinese quince medicinal extract 1.3%, green plum medicinal extract 1.5%, neohesperidin dihydrochalcone 0.4%, height
Former Rosa Damascana 0.1%, essential oil of tobaccos 1.8%, eastern Fructus Perillae quintessence oil 1.2%, glycerol 5%；Its surplus is triacetyl glycerine.
Each raw material is uniformly mixed to obtained light yellow liquid, as required cigarette filter-tip additive agent.
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
Snow mountain Radix Glycyrrhizae sweet ingredient 25%, acid Chinese quince medicinal extract 1.5%, green plum medicinal extract 1.2%, neohesperidin dihydrochalcone 0.4%, height
Former Rosa Damascana 0.08%, essential oil of tobaccos 1.8%, eastern Fructus Perillae quintessence oil 1.2%, glycerol 6%；Its surplus is triacetyl glycerine.
Each raw material is uniformly mixed to obtained 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 snow mountain Radix Glycyrrhizae sweet ingredient purification.It comments
Inhale the result shows that: compare with control sample, the dry sensation and irritant effects of additives of filter tip reduction cigarette smoking of the invention
Clearly, moreover it is possible to the salubrious moisture feeling of cigarette smoke, natural sweet tea sense are assigned, time sweet tea is lasting, pleasant impression is clean, and flue gas is softer,
Fragrance is more abundant, and the effect that cigarette suction comfort improves is obvious.
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 snow mountain Radix Glycyrrhizae sweet ingredient purification
It smokes panel test.Smoking result shows: comparing with control sample, additives of filter tip of the invention reduces dry sensation and the stimulation of cigarette smoking
Property effect clearly, moreover it is possible to assign the salubrious moisture feeling of cigarette smoke, natural sweet tea sense, return that sweet tea is lasting, pleasant impression is clean, flue gas is more
Soft, 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: snow mountain Radix Glycyrrhizae sweet ingredient 20-30%,
Acid Chinese quince medicinal extract 1.2-1.5%, green plum medicinal extract 1.2-1.5%, neohesperidin dihydrochalcone 0.2-0.4%, plateau rhodamine toner
Oily 0.05%-0.1%, essential oil of tobaccos 1.5%-2%, eastern Fructus Perillae quintessence oil 0.8-1.5%, glycerol 4-6%；Its surplus is three acetic acid
Glyceride.
2. according to cigarette filter-tip additive agent according to claim 1, which is characterized in that the snow mountain Radix Glycyrrhizae sweet ingredient is
Snow mountain Radix Glycyrrhizae sweet ingredient is dissolved in triacetyl glycerine and glycerol (wherein triacetyl glycerine and glycerol volume ratio are 90:10)
Solution.
3. cigarette filter-tip additive agent according to claim 1, which is characterized in that snow mountain Radix Glycyrrhizae sweet ingredient extraction side
Method 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. snow mountain Radix Glycyrrhizae is crushed to 30~50 mesh powders to be added in the ultrasonic extraction tank (1), with powder weight 2~3
80wt% EtOH Sonicate again extracts 30~50min of powder, is then forced through the filter bag (6) and extracting solution entrance is obtained by filtration
In concentration 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 50 that wherein Residual ethanol is gross mass~
Concentrate is obtained when 60wt%；
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
4~5 times of volume, then with 50~60wt% ethanol washing chromatographic column of 1~1.5 times of admission space of resin (13)；
3. the chromatographic column (18) 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 snow mountain Radix Glycyrrhizae sweet taste at
Point.
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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| Application Number | Priority Date | Filing Date | Title |
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| CN201811097929.5A CN109288125B (en) | 2018-09-20 | 2018-09-20 | Filter tip additive mainly containing refined radix glycyrrhizae preparata sweet components and preparation method thereof |
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| CN201811097929.5A CN109288125B (en) | 2018-09-20 | 2018-09-20 | Filter tip additive mainly containing refined radix glycyrrhizae preparata sweet components and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111635825A (en) * | 2020-05-18 | 2020-09-08 | 云南中烟工业有限责任公司 | Snow mountain liquorice essence for cigarette bead blasting, bead blasting prepared from snow mountain liquorice essence and cigarette |
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|---|---|
| CN109288125B (en) | 2021-01-29 |
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