CN109288125B - Filter tip additive mainly containing refined radix glycyrrhizae preparata sweet components and preparation method thereof - Google Patents
Filter tip additive mainly containing refined radix glycyrrhizae preparata sweet components and preparation method thereof Download PDFInfo
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- CN109288125B CN109288125B CN201811097929.5A CN201811097929A CN109288125B CN 109288125 B CN109288125 B CN 109288125B CN 201811097929 A CN201811097929 A CN 201811097929A CN 109288125 B CN109288125 B CN 109288125B
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Images
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Seasonings (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
本发明公开了一种卷烟滤嘴添加剂，包括如下重量成分：雪山甘草甜味成分20‑30％，酸木瓜浸膏1.2‑1.5％，青梅浸膏1.2‑1.5％，新橙皮苷二氢查尔酮0.2‑0.4％、高原玫瑰精油0.05％‑0.1％，烟草精油1.5％‑2％，东紫苏精油0.8‑1.5％，甘油4‑6％；其余量为三醋酸甘油酯。本发明还公开了所述雪山甘草甜味成分制备方法及用于卷烟滤嘴中降低卷烟抽吸干燥感和刺激性的用途。
The invention discloses an additive for a cigarette filter tip, comprising the following weight components: 20-30% of snow mountain licorice sweetness, 1.2-1.5% of sour papaya extract, 1.2-1.5% of green plum extract, neohesperidin dihydrochalcogenide Cherone 0.2-0.4%, plateau rose essential oil 0.05%-0.1%, tobacco essential oil 1.5%-2%, oriental perilla essential oil 0.8-1.5%, glycerin 4-6%; the balance is triacetin. The invention also discloses the preparation method of the snow-capped licorice sweet component and the use in the cigarette filter to reduce the dryness and irritation of cigarette smoking.
Description
Technical Field
The invention belongs to the technical field of cigarette additives, and particularly relates to a filter tip additive taking a refined sweet component of radix glycyrrhizae snow as a main component and a preparation method thereof, and application of the sweet component of radix glycyrrhizae snow in preparing the cigarette filter tip additive.
Background
Radix Glycyrrhizae in the form of powder is selected from Phlomis betonicoides Diels of Labiatae (Lamiaceae) genus Phlomis, and is also called radix Gentianae Macrophyllae, radix Ginseng alba, radix Panacis Quinquefolii, radix scrophulariae, radix Rumicis Japonici, radix scrophulariae, and radix Codonopsis Pilosulae. Distributed in the northwest, southwest Sichuan and eastern Tibet of Yunnan province. The root can be used as medicine for treating dyspepsia, abdominal distention, throat pain, traumatic injury, tuberculosis, pneumonia, and relieving various drug poisoning. The sweetness of the main sweet substance of the Xueshan liquorice, namely the cynanchum otophyllum glycoside, is 600 times that of the cane sugar, the sweetness is pure, the sweetness can be kept for about 1 hour, the aftertaste of the oral cavity is very comfortable, and the plant is widely distributed in Yunnan Lijiang, Shangri La, Nutgiang, the east of Tibet, the West of Sichuan and the like. Literature [ food industry, 2016, 37 (12): 142-145) adopts complex enzyme to carry out enzymolysis extraction on the dolichos japonicus, the enzymolysis liquid is concentrated, and amino acid is added to carry out Maillard reaction to prepare the tobacco flavor. The literature reports that the glycyrrhiza glabra extract prepared by subcritical extraction (CN201710198020.8) or heating reflux extraction (CN201610915435.8) is used as the cigarette filter stick additive, so that the sweet feeling of cigarette smoke can be effectively increased, and the cigarette smoking comfort is improved. However, the glycyrrhiza glabra contains bitter components (chem. pharm. Bull.,1983, 31(2):780-783) besides sweet components, and if the bitter components cannot be separated, the quality of the additive is not high, and the smoking taste of cigarette smoke is not pure after the additive is added into cigarette filters.
The invention provides a method for refining a sweet taste component of radix glycyrrhizae snow mountain by using reverse phase resin column chromatography, which aims at overcoming the defects of the prior art, can effectively remove bitter components by using the method, obtains a purer refined sweet taste component of radix glycyrrhizae snow mountain, and uses the obtained refined sweet taste component of radix glycyrrhizae snow mountain to prepare a filter tip additive, thereby solving the problems of smoking dryness and irritation of cigarettes and improving the smoking comfort.
Disclosure of Invention
The invention aims to provide a novel method for refining sweet components in the radix glycyrrhizae snow mountain by using reverse phase resin column chromatography, and a cigarette filter additive is prepared by depending on the sweet components in the refined radix glycyrrhizae snow mountain; the additive is added into the cigarette filter in the cigarette filter forming process, so that the dry feeling and irritation of the cigarette can be effectively reduced, and the smoking comfort of the cigarette is improved.
All percentages used herein are by weight unless otherwise indicated.
The purpose of the invention is realized by the following technical scheme.
The invention discloses a cigarette filter additive in a first aspect, which is characterized by comprising the following components in parts by weight: 20-30% of sweet component of the radix glycyrrhizae, 1.2-1.5% of fructus chaenomelis extract, 1.2-1.5% of green plum extract, 0.2-0.4% of neohesperidin dihydrochalcone, 0.05-0.1% of plateau rose essential oil, 1.5-2% of tobacco essential oil, 0.8-1.5% of perilla frutescens essential oil and 4-6% of glycerol; the rest is glycerol triacetate.
Preferably, the sweet component of the glycyrrhiza uralensis is a solution of the sweet component of the glycyrrhiza uralensis, which is dissolved in glycerol triacetate and glycerin (wherein the volume ratio of the glycerol triacetate to the glycerin is 90: 10).
Preferably, the method for extracting the sweet components of the glycyrrhiza uralensis fisch uses the following extraction device and refining device for extraction:
the extraction device comprises the following components:
an ultrasonic extraction tank 1 having a feed port 3 and a pressurizing port 4 at the upper part thereof, communicating with an extract liquid feed pump 2, and a first discharge port 11-1 at the lower part thereof;
-a filter bag 6;
-an air compressor 5;
a concentration tank 9, the lower part of which is provided with a second discharge port 11-2;
-a condenser 10;
-a solvent recovery tank 12;
the connection mode of each part is as follows:
the ultrasonic extraction tank 1 is communicated with an inlet at the upper part of the filter bag 6 through a first discharge hole 11-1, and the upper part of the ultrasonic extraction tank 1 is communicated with the air compressor 5 through the pressurizing hole 4; the outlet at the lower part of the filter bag 6 is communicated with the concentration tank 9, the upper part of the concentration tank 9 is communicated with the inlet of the condenser 10, and the outlet of the condenser 10 is communicated with the solvent recovery tank 12;
the refining device comprises the following components:
a chromatographic column 18, placed horizontally, filled with a resin 13, the outside of said resin 13 being fixed by a sieve plate 19;
an eluate fraction collection tank 16;
an effluent and wash liquor collection tank 17;
a four-way valve 14;
-a three-way valve 15;
the connection mode of each part is as follows:
one side sieve plate 19 of the chromatographic column 18 is communicated with one valve port of the four-way valve 14, and the other three valve ports of the four-way valve 14 are respectively: valve port a is communicated with the elution component collecting tank 16, valve port b is connected with the F pump, and valve port c is connected with the G pump; the sieve plate 19 on the other side of the chromatographic column 18 is communicated with one valve port of the three-way valve 15, and the other two valve ports of the three-way valve 15 are respectively: the valve port d of the valve is communicated with the effluent liquid and washing liquid collecting tank 17, and the valve port e of the valve is connected with the H pump;
the extraction method comprises the following steps:
crushing the snow mountain liquorice into powder of 30-50 meshes, adding the powder into an ultrasonic extraction tank 1, ultrasonically extracting the powder for 30-50 min by using 80wt% ethanol 2-3 times the weight of the powder, then pressurizing the powder, filtering the powder through a filter bag 6 to obtain an extracting solution, feeding the extracting solution into a concentration tank 9, washing filter residues by using 80wt% ethanol 0.5-0.8 times the weight of the powder, filtering out a washing solution, combining the extracting solution and the washing solution in the concentration tank 9, and concentrating the extracting solution and the washing solution under reduced pressure until the ethanol residue accounts for 50-60 wt% of the total mass to obtain a concentrated solution;
secondly, passing the concentrated solution obtained in the first step through a reversed-phase resin chromatographic column 18, wherein the volume of the concentrated solution is 4-5 times of the filling volume of the resin 13, and then washing the chromatographic column with 50-60 wt% ethanol, 1-1.5 times of the filling volume of the resin 13;
thirdly, eluting the chromatographic column 18 washed in the second step in the reverse direction by using 80wt% ethanol, wherein the volume of the 80wt% ethanol is 4-5 times of the filling volume of the resin; collecting eluate, and concentrating under reduced pressure until no solvent is present to obtain the sweet component of radix Glycyrrhizae in snow mountain.
Preferably, the resin 13 is BOSHI reverse phase resin, the diameter of the filling of the resin 13 is 1:2, and the particle size of the reverse resin is 35-75 μm.
The invention discloses the application of the cigarette filter additive in reducing the dry feeling and irritation of cigarettes in a second aspect.
Preferably, the evaluation method for reducing the cigarette smoking dryness and the irritation adopts the expression level of the cell AQP5 protein to evaluate the effect of the filter additive on reducing the cigarette smoking dryness and the irritation.
The method for extracting the sweet components from the cigarette filter additive and the radix glycyrrhizae sieboldii, the application of the cigarette filter additive, and the method for evaluating the dry feeling and the irritation of the cigarette filter additive are described in the following with reference to the accompanying drawings, and specifically the following steps are performed:
1. extraction and refining of sweet components of radix Glycyrrhizae in snow mountain
A. Sample extraction
The extraction process of radix Glycyrrhizae from snow mountain uses the device shown in figure 1. Pulverizing radix Glycyrrhizae into 30-50 mesh powder, and placing into ultrasonic extraction tank 1; then adding 80wt% ethanol which is 2-3 times of the weight of the powder; and (4) carrying out ultrasonic extraction for 30-50 min. After extraction, opening a first discharge port 11-1, starting an air compressor 5 to pressurize the ultrasonic extraction tank 1, and filtering the extracting solution through a filter bag 6 under the action of pressure; and after filtering, washing filter residues by using 80wt% ethanol with the weight 0.5-0.8 times of that of the powder, filtering out washing liquid, combining the extracting solution and the washing liquid, transferring the extracting solution and the washing liquid into a concentration tank 9, concentrating the extracting solution under reduced pressure until the residual quantity of the ethanol in the concentrated solution is 50-60 wt%, and stopping concentration for column chromatography separation. The solvent ethanol is cooled by a condenser 10 and then enters a solvent recovery tank 12.
B. Separating by column chromatography
The column chromatography separation process and device are shown in figure 2. The concentrated solution from the concentration tank 9 in fig. 1 is discharged from the second discharge port 11-2, and then enters the BOSHI reversed-phase resin chromatographic column 18 through the port b of the four-way valve 14, and then flows out through the port d of the three-way valve 15, and finally enters the effluent and washing solution collection tank 17. Wherein the diameter of the resin filled in the chromatographic column 18 is 1:2, the particle size of the resin is 35-75 μm, and the amount of the solution passing through the column is 4-5 times of the filling volume of the resin. And then washing the chromatographic column by using 25-30 wt% ethanol washing liquid with the volume 1-1.5 times of the resin filling volume, conveying the washing liquid through the chromatographic column 18 by using a G pump, and allowing the washing liquid to enter from an opening b of the four-way valve, flow out from an opening d of the three-way valve 15 after passing through the chromatographic column 18 and enter an effluent liquid and washing liquid collecting tank 17.
In the process, the sample solution passes through the chromatographic column 18 by using 50-60 wt% of ethanol, and the chromatographic column 18 is washed by using 50-60 wt% of ethanol, so that the sweet components and the bitter components in the snow mountain liquorice are effectively separated.
C. Elution and sample concentration of sweet components of radix glycyrrhizae koreanae
After the above column chromatography separation step is completed, the H pump in FIG. 2 is started, and the column is eluted in the reverse direction with 65 wt% ethanol, wherein the volume of 65 wt% ethanol is 4-5 times of the resin packing volume. In the process, eluent enters from the port e of the three-way valve 15 in the figure 2, passes through the chromatographic column 18 and then flows out from the port a of the four-way valve 14, and then enters the eluent component collecting tank 16.
Concentrating the eluent collected in the eluent collecting tank 16 under reduced pressure until no solvent is available to obtain the sweet component of the radix glycyrrhizae. Then dissolving the glycerol triacetate into glycerol triacetate to form a solution for later use; wherein the volume ratio of the glycerol triacetate to the glycerol is 90: 10.
2. Preparation of cigarette filter tip additive
The cigarette filter additive is prepared from the following raw materials in percentage by mass: c, 20-30% of the sweet component of the Yunnan Xueshan liquorice, 1.2-1.5% of the fructus chaenomelis extract, 1.2-1.5% of the green plum extract, 0.2-0.4% of neohesperidin dihydrochalcone, 0.05-0.1% of plateau rose essential oil, 1.5-2% of tobacco essential oil, 0.8-1.5% of east perilla essential oil and 4-6% of glycerin; the rest is glycerol triacetate. The light yellow liquid obtained by uniformly mixing the raw materials is the required cigarette filter additive. Wherein the sweet component of radix Glycyrrhizae is added in the form of solution of glycerol triacetate and glycerol (volume ratio of 90: 10).
The cigarette filter additive takes sweet components refined from the liquorice in the snow mountain as main raw materials. The sweet component refined from the glycyrrhiza uralensis from the snow mountain has not only pure sweet taste but also strong sweet feeling, the sweet taste can be kept for about 1h, and very comfortable sweet aftertaste can be given to the oral cavity.
The sour papaya extract and the green plum extract are extracted from Yunnan sour and sweet fruits, and are commonly used as food flavoring agents which are widely used for various beverages, soda water and candies, can endow the additive with pure sour taste, have strong sour flavor, can neutralize free nicotine in partial cigarette smoke, and effectively reduce the cigarette smoking irritation.
The neohesperidin dihydrochalcone is a sweetener with extremely high sweetness prepared by taking citrus peels as a raw material, the sweetness of the sweetener is 1800 times that of cane sugar, the taste is fresh and cool, the aftertaste is lasting, the sweetener has excellent effects of shielding bitter taste and covering offensive odor, and the sweet feeling of the additive can be increased by matching the sweetener with the sweet component of the glycyrrhiza uralensis, so that the sweetness is richer, fresh and natural.
The plateau rose essential oil, the perilla frutescens essential oil and the tobacco essential oil are all natural plant extracts. The plateau rose essential oil has the special faint scent and sweet scent of strong rose, thick and heavy scent texture, elegant and natural scent, and can endow cigarette smoke with elegant fresh and sweet scent. The perilla frutescens essential oil has fresh and sweet fragrance, has elegant green and grass sweet smell and cool taste, can effectively reduce the irritation of cigarette smoke and enrich the fragrance of the smoke. The tobacco absolute oil is rich in a large amount of tobacco aromatic components, can increase the original tobacco aroma characteristics of cigarette smoking, covers the miscellaneous gas of the cigarette and enables the tobacco aroma to be richer and more natural.
The glycerol has solubilization, can increase the solubility of acid and sweet components in the additive, and the fragrance components added in the formula can be kept stable, so as to increase the moistening feeling of cigarette smoking.
3. Biological evaluation of filter tip additive for reducing cigarette dry feeling and irritation
The filter tip reducing additive is evaluated by adopting a dryness reducing and body fluid generating model constructed by cell aquaporin 5(AQP 5). Firstly, saliva acinar cells are subjected to drug pretreatment to simulate a cell microenvironment when a xerosis syndrome occurs, then filter additives with different concentrations are adopted to stimulate the cells, the cells are fixed and permeable after stimulation is finished, an FITC-labeled AQP5 antibody is added for dyeing and labeling, a high content imaging system is used for observing the expression quantity of cell AQP5 protein after the filter additives are used for treatment, and the cell AQP5 protein is compared with a cell control sample which is not treated by the filter additives. The results show that: the filter tip additive can up-regulate the expression level of cell AQP5 protein, so that the filter tip additive has a good effect of promoting the secretion of saliva or body fluid, can improve the smoking feeling of cigarettes and reduce the irritation.
4. Filter tip addition and cigarette preparation
The filter tip additive takes glycerol triacetate as a medium. In the cigarette filter forming process, a filter additive is added to the cigarette filter. The cigarette to be added is a cigarette product 'purple cloud' or 'red camellia soft' of the Hongyun Honghe group, and is uniformly sprayed on the filter tow according to 6-8 w% of the weight of the filter tow to prepare a cigarette filter stick, then the cigarette filter stick is connected into a cigarette through a conventional cigarette roll to carry out sensory evaluation, and the same cigarette of the additive with the same formula without refining the sweet component of the radix glycyrrhizae uralensis is taken as a reference sample to carry out sensory evaluation. The results of the smoke panel test show that: compared with a control sample, the filter tip additive provided by the invention is added into a filter tip of a cigarette, so that the dryness and irritation of cigarette smoking are reduced, the effect is very obvious, the smoke of the cigarette can be endowed with fresh and moist feeling and natural sweet feeling, the aftertaste is lasting, the aftertaste is clean, the smoke is softer, and the fragrance is richer. The result shows that the filter tip additive has very obvious effect of improving the smoking comfort of cigarettes.
The invention has the beneficial effects that:
1. the filter tip additive takes the sweet component of the snow mountain liquorice as the main raw material, and the sweet taste is pure and natural.
2. The purification apparatus of the present invention comprises a reverse phase resin column, and the target component can be purified by using the chromatography reverse phase resin column. The BOSHI reversed-phase resin is a polystyrene-divinylbenzene copolymerization material, is designed based on the modern HPLC liquid chromatography separation technology, has smaller particles and higher chromatographic separation performance, and is used for separating, refining and purifying plant target components for the first time. Compared with the traditional bonded silica gel of reversed-phase column chromatography materials, the material has higher adsorption capacity, higher material stability and lower material cost. The reverse resin chromatographic column can be reused more than 6000 times, can keep good column efficiency, and has lower actual production cost than other column chromatographic separation processes.
3. The invention relates to an ultrasonic extraction device (shown as a figure 1) and an automatic column chromatography device (shown as a figure 2). Compared with the traditional reflux extraction process, the ultrasonic extraction process has the advantages that the energy consumption in the extraction process is reduced, and the extraction is more complete. Through automatic column chromatography technology, sample application, washing, elution all can be through numerical control valve control, can realize the automation mechanized operation of column chromatography separation, and production operation degree of automation is high, and the human cost is low.
4. The solvent used in the invention is ethanol, glycerol or glycerol triacetate and the like, which are all common additives for cigarettes, and the production process does not introduce harmful solvent residues; wherein, the solvent ethanol with large consumption can be recycled, the production process is safe and environment-friendly, and the generation consumption and the cost are low.
5. The application of the filter additive in the cigarette industry is easy to realize. In the process of forming a filter stick in cigarette production, glycerol triacetate is required to be added as a plasticizer in the formation of a cigarette filter, and the addition amount is 6-8% of the weight of a filter stick tow. The filter tip additive disclosed by the invention has the advantages that the problem of industrial application is considered in the design stage, and glycerol triacetate is adopted to prepare the additive in a targeted manner; the main component of the filter tip additive is triacetyl glycerine (accounting for about 95 wt% of the additive), so that the additive can replace the plasticizer triacetyl glycerine in the process of forming the cigarette filter tip, an additional procedure is required in the process of forming the filter tip, and the industrial application is very easy to realize.
6. The invention uses the Xueshan liquorice as a main raw material, and also adopts various selected natural plant extracts and monomer spices to blend the additive, so that the aroma richness of the filter tip additive is enriched and the effect of cigarette smoking comfort is improved through the synergistic effect of the extracts and the monomer spices and the sweet taste component of the Xueshan liquorice.
7. According to the invention, the dryness-reducing and body fluid-generating effects of the additive are evaluated by adopting the expression level of the up-regulated cell AQP5 protein, and the supplement is formed by the traditional artificial sensory evaluation, so that the objectivity of the effect evaluation of the filterable mouth additive is improved.
Drawings
FIG. 1 is a diagram of an apparatus for extracting a sample of radix Glycyrrhizae from the snow mountain.
FIG. 2 is a view of an apparatus for refining sweet components of radix Glycyrrhizae in the snow mountain.
The reference signs are: 1. an ultrasonic extraction tank; 2. an extract liquid conveying pump; 3. a feed inlet; 4. a pressurizing port; 5. an air compressor; 6. a filter bag; 7. an enamel interface; 8. a valve; 9. a concentration tank; 10. a condenser; 11-1, a first discharge port; 11-2 and a second discharge hole; 12. an ethanol recovery device; 13. a vacuum tube; 14. a four-way valve; 15. a three-way valve; 16 an eluted component collecting tank; 17. effluent and wash liquor collection tanks; 18. a chromatography column; 19. a sieve plate; F. f, a pump; G. a G pump; H. an H pump; a. a port a of the four-way valve; b. a port b of the four-way valve; c. a port c of the four-way valve; d. a port d of the three-way valve; e. and a port e of the three-way valve.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The raw materials and equipment used in the examples are commercially available or commonly used in the art, unless otherwise specified, and the methods in the examples are conventional in the art, unless otherwise specified.
Example 1: extraction and refining of sweet components of radix Glycyrrhizae in snow mountain
A. Sample extraction
As shown in figure 1, pulverizing radix Glycyrrhizae into 40 mesh powder, and placing into ultrasonic extraction tank; then adding 80wt% ethanol 2 times of the weight of the powder; ultrasonic extraction is carried out for 30min, after the ultrasonic extraction is finished, a discharge port 11-1 is opened, an air compressor is started to pressurize the interior of an ultrasonic extraction tank 1, and the extracting solution is filtered by a filter bag 6 under the action of pressure; after the filtration is completed, the filter residue is washed with 80wt% ethanol solution of which the weight is 0.5 times of the weight of the powder, the washing solution is filtered out, and the extracting solution and the washing solution are combined and transferred to a concentration tank 9. Concentrating the extractive solution and washing solution under reduced pressure until the residual amount of ethanol is 50 wt%, and separating by column chromatography.
B. Isolation of sweet taste component
As shown in FIG. 2, the concentrated solution discharged from the discharge port 11-2 of the concentration tank 9 was pumped through a BOSHI reverse phase resin column (diameter of packing resin of column: height: 1:2, particle diameter of reverse phase resin: 35 μm) by an F pump in FIG. 2, and the amount of the column-passing solution was 4 times the packing volume of the resin. In the process, the sample solution enters from the port b of the four-way valve in FIG. 2, passes through the chromatographic column 18 and then flows out from the port d of the three-way valve in FIG. 2; after passing through the column, 50 wt% ethanol with 1 time of the volume of the resin is used for washing the chromatographic column, the washing liquid is conveyed through the chromatographic column 18 by a pump G in the figure 2, and the washing liquid enters from the port c of the four-way valve in the figure 2 and flows out from the three-way valve d in the figure 2 after passing through the chromatographic column 18. In this process, the sample solution is passed through the column 18 with 50 wt% ethanol medium, and the column 18 is washed with 50 wt% ethanol.
C. Elution and concentration of sweet taste components
After the washing in the above step is completed, the H pump in FIG. 2 is started, and the column 18 is eluted in the reverse direction with 80wt% ethanol in a volume of 4 times the volume of the resin packed in the column. In the process, 80wt% of ethanol enters from a three-way valve e in the figure 2, flows out from a four-cylinder valve a after passing through a chromatographic column, enters an elution component collecting tank 16, and after elution is finished, eluent in the elution component collecting tank 16 is decompressed and concentrated to be dry without solvent, so that sweet components in the radix glycyrrhizae uralensis are obtained, and then are dissolved in a mixed solvent of triacetin and glycerol (the volume ratio of the triacetin to the glycerol is 90: 10).
Example 2: extraction and refining of sweet components of radix Glycyrrhizae in snow mountain
A. Sample extraction
As shown in figure 1, pulverizing radix Glycyrrhizae to 45 mesh powder, adding into ultrasonic extraction tank 1 via charging port 3, adding 80wt% ethanol 3 times of the powder into ultrasonic extraction tank 1, and ultrasonic extracting for 50 min. Opening a discharge port 11-1 after extraction, starting an air compressor 5 to pressurize the ultrasonic extraction tank 1, and filtering the extracting solution through a filter bag 6 under the action of pressure; after the filtration is completed, the filter residue is washed with 80wt% ethanol which is 0.8 times of the weight of the sample, the washing liquid is filtered out, and the extracting solution and the washing liquid are combined and transferred to a concentration tank 9. Concentrating the extractive solution and washing solution under reduced pressure until the residual amount of ethanol is 60wt%, and separating by column chromatography. The solvent ethanol is cooled by a condenser 10 and then enters a solvent recovery tank 12.
B. Isolation of sweet taste component
As shown in FIG. 2, the concentrated solution from the outlet 11-2 of the concentrating tank 9 was pumped through a BOSHI reversed-phase resin column 18 by a pump F in FIG. 2, the column 18 was filled with a resin 13, the diameter of the resin 13 was 1:2, the particle size of the resin 13 was 75 μm, and the amount of the solution passing through the column 18 was 5 times the volume of the resin. In the process, the sample solution enters from the port b of the four-way valve in FIG. 2, passes through the chromatographic column 18 and then flows out from the port d of the three-way valve in FIG. 2; after passing through the column, 60wt% ethanol with the volume 1.5 times that of the resin is used for washing the chromatographic column, the washing liquid is conveyed through the chromatographic column 18 by a pump G in the figure 2, and the washing liquid enters from an opening of a four-way valve c in the figure 2 and flows out from a three-way valve d in the figure 2 after passing through the chromatographic column 18. In this process, the sample solution is passed through the column 18 with 60wt% ethanol medium, and the column 18 is washed with 60wt% ethanol. The effluent and wash liquid enter the effluent and wash liquid collection tank 17.
C. Elution and concentration of sweet taste components
After the washing in the above step is completed, the H pump in FIG. 2 is started, and the column 18 is eluted in the reverse direction with 80wt% ethanol in a volume 5 times the volume of the column 18 filled with the resin 13. In the process, 80wt% of ethanol enters from a three-way valve e in the figure 2, flows out from a four-cylinder valve a after passing through a chromatographic column 18, enters an elution component collecting tank 16, and after elution is finished, eluent in the elution component collecting tank 16 is decompressed and concentrated to be dry without solvent, so that sweet components in the radix glycyrrhizae uralensis are obtained, and then are dissolved in a mixed solvent of triacetin and glycerol (the volume ratio of the triacetin to the glycerol is 90: 10).
Example 3: extraction and refining of sweet components of radix Glycyrrhizae in snow mountain
A. Sample extraction
As shown in figure 1, pulverizing radix Glycyrrhizae into 30 mesh powder, and placing into ultrasonic extraction tank; then 80wt% ethanol with 2.5 times of the weight of the powder is added into the ultrasonic extraction tank; ultrasonic extracting for 40 min. Opening a discharge port after extraction, starting an air compressor to pressurize the ultrasonic extraction tank, and filtering the extract through a filter bag under the action of pressure; after the filtration is completed, the filter residue is washed with 80wt% ethanol which is 0.6 times of the weight of the sample, the washing liquid is filtered out, and the extracting solution and the washing liquid are combined and transferred to a concentration tank 9. The extract and the washing solution were concentrated under reduced pressure until the residual amount of ethanol was 55 wt%, and subjected to column chromatography.
B. Isolation of sweet taste component
As shown in FIG. 2, the concentrated solution discharged from the discharge port 11-2 of the concentration tank 9 was pumped through a BOSHI reverse phase resin column (diameter of packed resin in the column: height: 1:2, particle diameter of reverse phase resin: 50 μm) by an F pump in FIG. 2, and the amount of the column-passing solution was 4 times the packed volume of the resin. In the process, the sample solution enters from the port b of the four-way valve in FIG. 2, passes through the chromatographic column 18 and then flows out from the port d of the three-way valve in FIG. 2; after passing through the column, 55 wt% ethanol with 1 time of the volume of the resin is used for washing the chromatographic column, the washing liquid is conveyed through the chromatographic column 18 by a pump G in the figure 2, and the washing liquid enters from the port c of the four-way valve in the figure 2 and flows out from the three-way valve d in the figure 2 after passing through the chromatographic column 18. In this process, the sample solution is passed through the column 18 with 55 wt% ethanol medium, and the column 18 is washed with 55 wt% ethanol.
C. Elution and concentration of sweet taste components
After the washing in the above step is completed, the H pump in FIG. 2 is started, and the column 18 is eluted in the reverse direction with 80wt% ethanol in a volume of 5 times the volume of the resin packed in the column. In the process, 80wt% of ethanol enters from a three-way valve e in the figure 2, flows out from a four-cylinder valve a after passing through a chromatographic column, enters an elution component collecting tank 16, and after elution is finished, eluent in the elution component collecting tank 16 is decompressed and concentrated to be dry without solvent, so that sweet components in the radix glycyrrhizae uralensis are obtained, and then are dissolved in a mixed solvent of triacetin and glycerol (the volume ratio of the triacetin to the glycerol is 90: 10).
Example 4: preparation of filter tip additive
The cigarette filter additive is prepared from the following raw materials in percentage by mass: 20% of the sweet component of the glycyrrhiza uralensis from the snow mountain, 1.2% of the extract of the papaya, 1.2% of the extract of the green plum, 0.2% of neohesperidin dihydrochalcone, 0.05% of the essential oil of the plateau rose, 1.5% of the essential oil of tobacco, 0.8% of the essential oil of the oriental perilla and 4% of glycerin; the rest is glycerol triacetate. The light yellow liquid obtained by uniformly mixing the raw materials is the required cigarette filter additive.
Example 5: preparation of filter tip additive
The cigarette filter additive is prepared from the following raw materials in percentage by mass: 30% of the refined sweet component of the glycyrrhiza uralensis from the snow mountain obtained in the embodiment 2, 1.3% of the extract of the papaya, 1.5% of the extract of the green plum, 0.4% of neohesperidin dihydrochalcone, 0.1% of the essential oil of the plateau rose, 1.8% of the essential oil of tobacco, 1.2% of the essential oil of the east perilla and 5% of glycerin; the rest is glycerol triacetate. The light yellow liquid obtained by uniformly mixing the raw materials is the required cigarette filter additive.
Example 6: preparation of filter tip additive
The cigarette filter additive is prepared from the following raw materials in percentage by mass: 25% of the sweet component of the Yunnan Xueshan liquorice obtained in the embodiment 3, 1.5% of the papaya extract, 1.2% of the green plum extract, 0.4% of neohesperidin dihydrochalcone, 0.08% of plateau rose essential oil, 1.8% of tobacco essential oil, 1.2% of eastern perilla essential oil and 6% of glycerin; the rest is glycerol triacetate. The light yellow liquid obtained by uniformly mixing the raw materials is the required cigarette filter additive.
Example 7: biological evaluation of filter additives
Any of the filter additives prepared in examples 4-6 was subjected to a biological evaluation test for reducing the irritation of cigarettes, which comprises the following steps:
the filter additive disclosed by the invention is evaluated by adopting a dryness-reducing and body-fluid-generating model constructed by cell aquaporin 5(AQP 5). The method comprises the steps of carrying out medicine pretreatment on salivary acinar cells to simulate a cell microenvironment when xerosis syndrome occurs, then adopting filter additives with different concentrations to stimulate the cells, fixing and permeating the cells after stimulation is finished, adding an FITC-labeled AQP5 antibody for dyeing and labeling, observing the expression quantity of cell AQP5 protein after filter additives are used for treatment by a high content imaging system, and comparing the expression quantity with a cell control sample which is not treated by the filter additives. The results show that: the filter tip additive can up-regulate the expression level of cell AQP5 protein, so that the filter tip additive has a good effect of promoting the secretion of saliva or body fluid, can improve the smoking feeling of cigarettes and reduce the dryness and irritation.
Example 8: application of filter tip additive in cigarette
The filter additive in example 4 was used for the effect test of cigarette filter, and the test conditions were as follows:
the cigarette for adding the additive is the cigarette 'purple cloud' of the Hongyun river group, the additive is uniformly sprayed on the filter tow according to 6 percent of the weight of the filter tow to prepare a filter rod, then the filter rod is rolled to prepare the cigarette for sensory evaluation, and the same cigarette of the additive with the same formula without refining the sweet component of the glycyrrhiza uralensis is taken as a control sample for sensory evaluation. The results of the smoke panel test show that: compared with a control sample, the filter tip additive disclosed by the invention has very obvious effects of reducing the dryness and irritation of cigarette smoking, can endow the cigarette with fresh and moist smoke and natural sweet feeling, and has the advantages of lasting sweet return, clean aftertaste, softer smoke, richer fragrance and obvious effect of improving the cigarette smoking comfort.
Example 9: application of filter tip additive in cigarette
The filter additive in example 6 was used for the effect test of cigarette filter, and the test conditions were as follows:
the additive is uniformly sprayed on the filter tow according to 6 percent of the weight of the filter tow to prepare a filter rod, then the filter rod is prepared into a cigarette through rolling and splicing, and sensory evaluation is carried out, and the same cigarette of the additive with the same formula without refining the sweet component of the radix glycyrrhizae rubra in the Xueshan is taken as a reference sample to carry out sensory evaluation. The results of the smoke panel test show that: compared with a control sample, the filter tip additive disclosed by the invention has very obvious effects of reducing the dryness and irritation of cigarette smoking, can endow the cigarette with fresh and moist smoke and natural sweet feeling, and has the advantages of lasting sweet return, clean aftertaste, softer smoke, richer fragrance and obvious effect of improving the cigarette smoking comfort.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the present invention, and these changes and modifications are within the scope of the present invention as defined in the appended claims.
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| JP3829718B2 (en) * | 2002-01-08 | 2006-10-04 | 株式会社島津製作所 | High performance liquid chromatograph |
| CN101029071B (en) * | 2007-04-05 | 2010-05-19 | 上海交通大学 | Method for preparing high-purity mogroside V from Luo Han Guo |
| CN101062077B (en) * | 2007-06-18 | 2011-04-06 | 石任兵 | Method for preparing stevia whole stevioside and stevia whole flavone at the same time |
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| CN104672205A (en) * | 2013-12-03 | 2015-06-03 | 刘群秀 | Compound used as food sweetener |
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| CN107583575A (en) * | 2016-07-10 | 2018-01-16 | 青岛科技大学 | A kind of preparation of stable type flores aurantii flavor flavouring essence for tobacco and purposes |
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