CN105001350A - Flash extraction method for rabdosia rubescens polysaccharide and application of method in cigarettes - Google Patents
Flash extraction method for rabdosia rubescens polysaccharide and application of method in cigarettes Download PDFInfo
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Abstract
The invention discloses a flash extraction method for rabdosia rubescens polysaccharide and application of the method in cigarettes. Firstly, rabdosia rubescens is smashed into powder, water is added and mixed evenly, the obtained material is arranged in a flash extractor for extraction, an extracting solution is centrifuged to obtain liquid supernatant; flash concentration is carried out on the liquid supernatant, and ethyl alcohol is added into the concentrated solution to carry out treatment to obtain precipitate; the precipitate is dissolved by adding water, deproteinization is carried out on the obtained solution by adopting a Sevage method, the solution after deproteinization is concentrated, and the concentrated solution is dried to obtain rabdosia rubescens crude polysaccharide; the crude polysaccharide is separated and purified through DEAE-Celluose gel chromatographic columns and Sephadex G200 gel chromatographic columns to obtain refined rabdosia rubescens polysaccharide. High purity rabdosia rubescens polysaccharide can be obtained through the method, operation is simple, cost is low, and the extract time is short. Experiments show that when the extracted rabdosia rubescens polysaccharide is applied to the cigarettes as humectant, the irritation and miscellaneous odors of the cigarettes can be lowered, and the mellow and full feeling and the comfort ability of the cigarettes are improved.
Description
Technical field
The present invention relates to a kind of extracting method and application thereof of effective components in plants, be specifically related to a kind of homogenate extraction method of Rabdosia rubescens polysaccharide and the application in cigarette thereof.
Background technology
Usually need to add one or more humectants to play the effect improving cigarette physics humid keeping performance and degrading resistance property in production of cigarettes.Simultaneously, the moisture that the use of humectant can make cigarette keep in flue gas when different zones environment is consumed, reduce the dry sensation of flue gas in smoking property of cigarette process and pungent sense, ensure the suction quality of cigarette, ensure that Cigarette design person is to the transmission of relaxation, comfort and satisfaction during cigarette smoking.The polyhydroxy substances such as glycerine, propylene glycol, sorbyl alcohol are mainly adopted to be humectant in current China cigarette industry, the object of this type of humectant is used to be to maintain the water ratio of pipe tobacco in the course of processing, improve the resist processing of pipe tobacco, but humectant is for the maintenance of cigarette product water ratio, the improvement effect of sucking comfort level is not ideal.Vast territory and abundant resources in China, and floristics is various, and contained effective constituent also respectively has feature, for the exploitation of Novel tobacco humectant provides rich in natural resources.Vegetable polysaccharides is polymerized by a large amount of monose, and containing a large amount of hydroxyls, its a large amount of hydroxyl can form hydrogen bond with water molecules, thus makes polysaccharide have stronger water-holding power.Natural plant polyose abundance, its development & application enriches one of cigarette additive resource, the effective way improving Sensory Quality of Cigarette.
Rabdosia rubescens is the herb of Labiatae Rabdosia plant " fork of cracking rice ", has stronger antitumor, antibacterial, anti-inflammatory analgesic action, and its complete stool has relief of symptoms to the esophageal carcinoma, cardiac cancer, mammary cancer, the rectum cancer, leukemia etc. and extends the effect of survival time.In Rabdosia rubescens, main chemical compositions is except kaurene class diterpene, also has triterpene, flavones and the chemical composition such as phenolic acid, polysaccharide.At present about the application of Rabdosia rubescens polysaccharide to concentrate anti-oxidant and antitumor etc. in, there is not been reported for the application on tobacco.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of homogenate extraction method of Rabdosia rubescens polysaccharide and the application in cigarette thereof.Utilize homogenate extraction method of the present invention can obtain the higher Rabdosia rubescens polysaccharide of purity, and simple to operate, cost is low, extraction time is short.The Rabdosia rubescens polysaccharide utilizing the present invention to extract to obtain can be applied in cigarette.The experiment proved that, the Rabdosia rubescens polysaccharide of extraction is applied in cigarette as humectant, the pungency of cigarette and assorted gas can be reduced, the mellow and full sense of raising cigarette and comfortableness etc.
In order to solve the problem, the technical scheme that the present invention takes is:
The invention provides a kind of homogenate extraction method of Rabdosia rubescens polysaccharide, described extracting method comprises the following steps:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder, then add distilled water mixing, the solid-liquid ratio of gained mixture is 15 ~ 25:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, obtain extracting solution;
C, step b gained extracting solution is carried out centrifugal, obtain supernatant liquor;
D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time supernatant liquor, merge twice gained supernatant liquor;
E, adopt flash thickener to concentrate steps d gained supernatant liquor, obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 60 ~ 80%, carries out alcohol precipitation, is precipitated thing after standing, centrifugal;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 10 ~ 50mg/mL solution, by Sevage ordinary method deproteination matter, Rabdosia rubescens polysaccharide soln after deproteination matter takes flash thickener to concentrate, gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides;
H, step g gained Rabdosia rubescens Crude polysaccharides is added distilled water be mixed with Crude polysaccharides solution, then adopt DEAE-Celluose gel chromatographic columns to be separated, the liquid collecting main chromatographic peak carries out freeze-drying; Solid after obtained freeze-drying is adopted the NH of 0.05mol/L
4hCO
3solubilize, gained solution adopts Sephadex G200 gel chromatographic columns to be again separated, and collects main chromatographic peak liquid and carries out freeze-drying, obtain refining Rabdosia rubescens polysaccharide solid after freeze-drying.
According to the homogenate extraction method of above-mentioned Rabdosia rubescens polysaccharide, extraction conditions when extracting in step b is: Extracting temperature is 50 ~ 70 DEG C, under 15000 ~ 20000 turns/min, extract 2 ~ 3min.
According to the homogenate extraction method of above-mentioned Rabdosia rubescens polysaccharide, condition time centrifugal in step c, f is: at 4 DEG C, centrifugal 8 ~ 10min under 8000 ~ 10000 turns/min condition.
According to the homogenate extraction method of above-mentioned Rabdosia rubescens polysaccharide, condition time concentrated in step e, g is: vacuum tightness be 0.08 ~ 0.098MPa, under temperature is the condition of 70 ~ 80 DEG C, concentrated 20 ~ 25s.
According to the homogenate extraction method of above-mentioned Rabdosia rubescens polysaccharide, the condition left standstill in step f is leave standstill 24h under 4 DEG C of conditions.
According to the homogenate extraction method of above-mentioned Rabdosia rubescens polysaccharide, the specification of DEAE-Celluose gel chromatographic columns is 5.0 × 50cm; When adopting DEAE-Celluose gel chromatographic columns to be separated, with the NaCl solution of 0.5mol/L for moving phase, flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method;
The specification of Sephadex G200 gel chromatographic columns is 5.0 × 50cm, when adopting Sephadex G200 gel chromatographic columns to be separated, with the NH of 0.05mol/L
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method.
A kind of application of Rabdosia rubescens polysaccharide in cigarette utilizing aforesaid method to extract.
According to the above-mentioned application of Rabdosia rubescens polysaccharide in cigarette, consumption when Rabdosia rubescens polysaccharide is applied in cigarette accounts for 0.005 ~ 0.1% of tobacco quality.
When applying in cigarette, addition manner is evenly be sprayed onto in pipe tobacco after dilute with water, and polysaccharide add-on is 0.005 ~ 0.1% of tobacco quality.
positive beneficial effect of the present invention:
1, utilize extracting and purifying method of the present invention can obtain highly purified refining Rabdosia rubescens polysaccharide, and be applied to cigarette, the pungency of cigarette and assorted gas can be reduced, improve mellow and full sense and the comfortableness of cigarette.When applying in cigarette, addition manner is evenly be sprayed onto in pipe tobacco after dilute with water, and polysaccharide add-on is 0.005 ~ 0.1% of tobacco quality.
2, compared to the prior art homogenate extraction method of the present invention, mainly contains following remarkable advantage:
A, employing homogenate extraction method of the present invention extract Rabdosia rubescens polysaccharide, can shorten extraction time, improve extraction yield.
B, employing gel chromatography column chromatography for separation purifying twice, obtain highly purified refining Rabdosia rubescens polysaccharide.
C, extraction process of the present invention are easy, and equipment operation and maintenance cost is low.Be beneficial to the structural integrity and biological activity that keep polysaccharide.
D, process experiment prove, the Rabdosia rubescens polysaccharide that the present invention extracts is to the humectation successful of tobacco product.
embodiment:
Below in conjunction with embodiment, set forth the present invention further, but do not limit content of the present invention.
Embodiment 1:
The homogenate extraction method of Rabdosia rubescens polysaccharide of the present invention, its detailed step is as follows:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder 100g, then add distilled water mixing, the solid-liquid ratio of gained mixture is 18:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, and Extracting temperature is 50 DEG C, extracts 2min, obtain extracting solution under 20000 turns/min;
C, by step b gained extracting solution at 4 DEG C, centrifugal 10min under 8000 turns/min condition, obtain supernatant liquor; D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time
Supernatant liquor, merges twice gained supernatant liquor;
E, steps d gained supernatant liquor adopted flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 80 DEG C, concentrated 20s), obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 60%, carries out alcohol precipitation, leaves standstill 24h under 4 DEG C of conditions, carries out centrifugal (at 4 DEG C, centrifugal 10min under 8000 turns/min condition), be precipitated thing after leaving standstill;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 10mg/mL solution, by Sevage ordinary method deproteination matter, Rabdosia rubescens polysaccharide soln after deproteination matter take flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 80 DEG C, concentrated 20s), gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides 3.10g, and yield is 3.10%;
H, get gained Rabdosia rubescens Crude polysaccharides 1.0g distilled water and dissolve, Crude polysaccharides solution after dissolving adopts DEAE-Celluose gel chromatographic columns (5.0 × 50cm) to be separated, with the NaCl solution of 0.5mol/L for moving phase, flow velocity is 2.0mL/min, with Phenol-sulphate acid method, chromatographic solution is developed the color, collect main chromatographic peak liquid, carry out freeze-drying; Then by the NH of freeze-drying gained solid 0.05mol/L
4hCO
3solubilize, is separated with Sephadex G200 gel chromatographic columns (5.0 × 50cm), again with the NH of 0.05mol/L
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method, collects main chromatographic peak liquid and carries out freeze-drying, and obtain refining Rabdosia rubescens polysaccharide solid 260mg, yield is 26.0%.
Embodiment 2:
The homogenate extraction method of Rabdosia rubescens polysaccharide of the present invention, its detailed step is as follows:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder 100g, then add distilled water mixing, the solid-liquid ratio of gained mixture is 20:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, and Extracting temperature is 60 DEG C, extracts 3min, obtain extracting solution under 15000 turns/min;
C, by step b gained extracting solution at 4 DEG C, centrifugal 10min under 8000 turns/min condition, obtain supernatant liquor; D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time
Supernatant liquor, merges twice gained supernatant liquor;
E, steps d gained supernatant liquor adopted flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 70 DEG C, concentrated 22s), obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 70%, carries out alcohol precipitation, leaves standstill 24h under 4 DEG C of conditions, carries out centrifugal (at 4 DEG C, centrifugal 10min under 8000 turns/min condition), be precipitated thing after leaving standstill;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 20mg/mL solution, by Sevage ordinary method deproteination matter, Rabdosia rubescens polysaccharide soln after deproteination matter take flash thickener carry out concentrating (vacuum tightness be 0.09MPa, under temperature is the condition of 70 DEG C, concentrated 22s), gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides 2.87g, and yield is 2.87%;
H, get gained Rabdosia rubescens Crude polysaccharides 1.0g distilled water and dissolve, Crude polysaccharides solution after dissolving adopts DEAE-Celluose gel chromatographic columns (5.0 × 50cm) to be separated, with 0.5mol/L NaCl solution for moving phase, flow velocity is 2.0mL/min, with Phenol-sulphate acid method, chromatographic solution is developed the color, collect main chromatographic peak liquid, carry out freeze-drying; Then by the NH of freeze-drying gained solid 0.05mol/L
4hCO
3solubilize, is separated with Sephadex G200 gel chromatographic columns (5.0 × 50cm), again with 0.05mol/L NH
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method, collects main chromatographic peak liquid and carries out freeze-drying, obtains refining Rabdosia rubescens polysaccharide solid 220mg, yield 22.0%.
Embodiment 3:
The homogenate extraction method of Rabdosia rubescens polysaccharide of the present invention, its detailed step is as follows:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder 100g, then add distilled water mixing, the solid-liquid ratio of gained mixture is 22:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, and Extracting temperature is 70 DEG C, extracts 3min, obtain extracting solution under 18000 turns/min;
C, by step b gained extracting solution at 4 DEG C, centrifugal 8min under 10000 turns/min condition, obtain supernatant liquor; D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time
Supernatant liquor, merges twice gained supernatant liquor;
E, steps d gained supernatant liquor adopted flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 75 DEG C, concentrated 25s), obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 80%, carries out alcohol precipitation, leaves standstill 24h under 4 DEG C of conditions, carries out centrifugal (at 4 DEG C, centrifugal 8min under 10000 turns/min condition), be precipitated thing after leaving standstill;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 30mg/mL solution, by Sevage ordinary method deproteination matter, Rabdosia rubescens polysaccharide soln after deproteination matter take flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 75 DEG C, concentrated 25s), gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides 3.32g, and yield is 3.32%;
H, get gained Rabdosia rubescens Crude polysaccharides 1.0g distilled water and dissolve, Crude polysaccharides solution after dissolving adopts DEAE-Celluose gel chromatographic columns (5.0 × 50cm) to be separated, with the NaCl solution of 0.5mol/L for moving phase, flow velocity is 2.0mL/min, with Phenol-sulphate acid method, chromatographic solution is developed the color, collect main chromatographic peak liquid, carry out freeze-drying; Then by the NH of freeze-drying gained solid 0.05mol/L
4hCO
3solubilize, is separated with Sephadex G200 gel chromatographic columns (5.0 × 50cm), again with the NH of 0.05mol/L
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method, collects main chromatographic peak liquid and carries out freeze-drying, obtains refining Rabdosia rubescens polysaccharide solid 268mg, yield 26.8%.
Embodiment 4:
The homogenate extraction method of Rabdosia rubescens polysaccharide of the present invention, its detailed step is as follows:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder 100g, then add distilled water mixing, the solid-liquid ratio of gained mixture is 19:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, and Extracting temperature is 55 DEG C, extracts 2min, obtain extracting solution under 18000 turns/min;
C, by step b gained extracting solution at 4 DEG C, centrifugal 9min under 9000 turns/min condition, obtain supernatant liquor;
D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time supernatant liquor, merge twice gained supernatant liquor;
E, steps d gained supernatant liquor adopted flash thickener carry out concentrating (vacuum tightness be 0.09MPa, under temperature is the condition of 75 DEG C, concentrated 20s), obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 65%, carries out alcohol precipitation, leaves standstill 24h under 4 DEG C of conditions, carries out centrifugal (at 4 DEG C, centrifugal 9min under 9000 turns/min condition), be precipitated thing after leaving standstill;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 40mg/mL solution, by Sevage ordinary method deproteination matter, Rabdosia rubescens polysaccharide soln after deproteination matter take flash thickener carry out concentrating (vacuum tightness be 0.09MPa, under temperature is the condition of 75 DEG C, concentrated 20s), gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides 3.00g, and yield is 3.00%;
H, get Rabdosia rubescens Crude polysaccharides 1.0g distilled water and dissolve, Crude polysaccharides solution after dissolving adopts DEAE-Celluose gel chromatographic columns (5.0 × 50cm) to be separated, with the NaCl solution of 0.5mol/L for moving phase, flow velocity is 2.0mL/min, with Phenol-sulphate acid method, chromatographic solution is developed the color, collect main chromatographic peak liquid, carry out freeze-drying; Then by the NH of freeze-drying gained solid 0.05mol/L
4hCO
3solubilize, is separated with Sephadex G200 gel chromatographic columns (5.0 × 50cm), again with the NH of 0.05mol/L
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method, collects main chromatographic peak liquid and carries out freeze-drying, obtains refining Rabdosia rubescens polysaccharide solid 225mg, yield 22.5%.
Embodiment 5:
The homogenate extraction method of Rabdosia rubescens polysaccharide of the present invention, its detailed step is as follows:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder 100g, then add distilled water mixing, the solid-liquid ratio of gained mixture is 20:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, and Extracting temperature is 65 DEG C, extracts 2min, obtain extracting solution under 20000 turns/min;
C, by step b gained extracting solution at 4 DEG C, centrifugal 8min under 10000 turns/min condition, obtain supernatant liquor; D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time
Supernatant liquor, merges twice gained supernatant liquor;
E, steps d gained supernatant liquor adopted flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 70 DEG C, concentrated 20s), obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 75%, carries out alcohol precipitation, leaves standstill 24h under 4 DEG C of conditions, carries out centrifugal (at 4 DEG C, centrifugal 8min under 10000 turns/min condition), be precipitated thing after leaving standstill;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 50mg/mL solution, by Sevage ordinary method deproteination matter, polysaccharide soln after deproteination matter take flash thickener carry out concentrating (vacuum tightness be 0.08MPa, under temperature is the condition of 70 DEG C, concentrated 20s), gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides 3.53g, and yield is 3.53%;
H, get gained Rabdosia rubescens Crude polysaccharides 1.0g distilled water and dissolve, Crude polysaccharides solution after dissolving adopts DEAE-Celluose gel chromatographic columns (5.0 × 50cm) to be separated, with the NaCl solution of 0.5mol/L for moving phase, flow velocity is 2.0mL/min, with Phenol-sulphate acid method, chromatographic solution is developed the color, collect main chromatographic peak liquid, carry out freeze-drying; Then by the NH of freeze-drying gained solid 0.05mol/L
4hCO
3solubilize, is separated with Sephadex G200 gel chromatographic columns (5.0 × 50cm), again with the NH of 0.05mol/L
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method, collects main chromatographic peak liquid and carries out freeze-drying, obtains refining Rabdosia rubescens polysaccharide solid 279mg, yield 27.9%.
Embodiment 6:
Take according to the ratio accounting for tobacco quality 0.001% the Rabdosia rubescens polysaccharide that embodiment 1 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas slightly softens, other effect not obvious (referring to table 3).
Embodiment 7:
Take according to the ratio accounting for tobacco quality 0.005% the Rabdosia rubescens polysaccharide that embodiment 1 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas slightly becomes mellow and full, soft, and comfortable taste slightly promotes (referring to table 3).
Embodiment 8:
Take according to the ratio accounting for tobacco quality 0.01% the Rabdosia rubescens polysaccharide that embodiment 1 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste slightly increases, and assorted gas and pungency slightly reduce (referring to table 3).
Embodiment 9:
Take according to the ratio accounting for tobacco quality 0.05% the Rabdosia rubescens polysaccharide that embodiment 1 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas obviously becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste promotes, and assorted gas and pungency reduce (referring to table 3).
Embodiment 10:
Take according to the ratio accounting for tobacco quality 0.1% the Rabdosia rubescens polysaccharide that embodiment 1 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas obviously becomes mellow and full, soft, and return sweet sense obviously, comfortable taste is good, assorted gas and pungency low (referring to table 3).
Embodiment 11:
Take according to the ratio accounting for tobacco quality 0.2% the Rabdosia rubescens polysaccharide that embodiment 1 obtains, then add distilled water obtain solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, pungency strengthens, and pleasant impression is deteriorated, and has residual (referring to table 3).
Embodiment 12:
Take according to the ratio accounting for tobacco quality 0.01% the Rabdosia rubescens polysaccharide that embodiment 2 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste slightly increases, and assorted gas and pungency slightly reduce.
Embodiment 13:
Take according to the ratio accounting for tobacco quality 0.05% the Rabdosia rubescens polysaccharide that embodiment 3 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas obviously becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste promotes, and assorted gas and pungency reduce.
Embodiment 14:
Take according to the ratio accounting for tobacco quality 0.1% the Rabdosia rubescens polysaccharide that embodiment 4 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas obviously becomes mellow and full, soft, and it is obvious to return sweet sense, and comfortable taste is good, assorted gas and pungency low.
Embodiment 15:
Take according to the ratio accounting for tobacco quality 0.05% the Rabdosia rubescens polysaccharide that embodiment 5 obtains, then add distilled water and be mixed with solution, this Rabdosia rubescens polysaccharide soln is evenly sprayed onto on pipe tobacco, rolls into cigarette after balance and smoke panel test.Smoking result shows, flue gas obviously becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste promotes, and assorted gas and pungency reduce.
application test: the application of Rabdosia rubescens polysaccharide in tobacco
the mensuration of inventive samples moisturizing rate:take Rabdosia rubescens polysaccharide prepared by embodiment 1, be mixed with distilled water the aqueous solution that massfraction is 5%; Put into the climatic chamber that temperature is (22 ± 1) DEG C, humidity is (40 ± 2) %.Meanwhile, compare with the distilled water of equivalent and 5% aqueous solution of propylene glycol.Timing measures the quality of each sample, according to the moisturizing rate of this sample of mathematic interpolation.Rabdosia rubescens polysaccharide, propylene glycol solution under temperature 22 DEG C, humidity 40% condition moisturizing rate over time curve refer to table 1.Result shows: relative to distilled water, propylene glycol control group, and Rabdosia rubescens polysaccharide obviously can both slow down the speed of moisture loss at day part, significantly improves moisturizing rate.
。
inventive samples physics humid keeping performance is tested:take a certain amount of blank pipe tobacco, put into the climatic chamber that temperature is (22 ± 1) DEG C, humidity is (60 ± 2) % and balance 48h.Take a certain amount of Rabdosia rubescens polysaccharide of the present invention, being made into massfraction with distilled water is 5% aqueous solution, evenly be sprayed onto (polysaccharide quality: tobacco quality=1:200) in the tobacco sample of overbalance, contrast with the propylene glycol solution of the distilled water of equivalent and same concentrations.These 3 groups of pipe tobaccos are placed in the climatic chamber that temperature is (22 ± 1) DEG C, humidity is (60 ± 2) % and balance 48h.By the 3 groups of tobacco sample balanced, often group is divided into 2 parts, is placed in weighing disk.Wherein, 1 increment product put into the baking oven of 105 DEG C, are dried to sample constant weight, weigh, according to the change of front and back quality, draw the initial aqueous rate of each application of sample pipe tobacco after cooling.Often organize another 1 increment product, put into temperature after precise for (22 ± 1) DEG C, humidity is in the climatic chamber of (40 ± 2) %.Timing weighs pipe tobacco.The instant water ratio of calculation sample, investigates the physics humectation effect of humectant.Result (referring to table 2) shows: add polysaccharide humectant with propylene glycol compared with blank pipe tobacco, and moisture loss is relatively slower, and the humectation ability of polysaccharide is better than propylene glycol, has good physics humid keeping performance.
。
inventive samples sense organ humid keeping performance is tested:be taken at temperature (22 ± 1) DEG C, under relative humidity (60 ± 2) % condition, some parts of Guizhou C3F thin material pipe tobacco after balance 48h, take Rabdosia rubescens polysaccharide and add the least possible distilled water according to accounting for tobacco quality 0.001%, 0.005%, 0.01%, 0.05%, 0.1%, 0.2% and be mixed with solution, spray equably with micro sprayer and be added on above-mentioned pipe tobacco.At temperature (40 ± 1) DEG C, 4 h are balanced by adding the pipe tobacco after sample, water ratio (12.5 ± 0.5) % is dried to again at (100 ± 1) DEG C, roll into cigarette with cigarette-roller and put into temperature (22 ± 1) DEG C, relative humidity is, after descending balance 48 h in the climatic chamber of (60 ± 2) %, smoked panel test by panel of experts.Control sample is that same level single-tobacco-typed cigarette, balances 48h equally under uniform temp, same humidity with source.Smoking result refers to table 3.
。
As can be seen from sensory evaluating smoking's result of table 3, the Main Function of Rabdosia rubescens polysaccharide to cigarette shows as and makes flue gas obviously become mellow and full, soft, and comfortable taste promotes, and has and falls assorted and reduce irritating effect.When the consumption of Rabdosia rubescens polysaccharide is less time, little to cigarette effect, time consumption reaches 0.2%, pungency strengthens, and consumption is 0.1% time, and flue gas obviously becomes mellow and full, soft, and it is obvious to return sweet sense, and comfortable taste is good, assorted gas and pungency low.Therefore, the Optimum of Rabdosia rubescens polysaccharide is 0.005 ~ 0.1% of tobacco quality.
Claims (8)
1. a homogenate extraction method for Rabdosia rubescens polysaccharide, is characterized in that, described extracting method comprises the following steps:
A, Rabdosia rubescens is ground into 40 ~ 60 object powder, then add distilled water mixing, the solid-liquid ratio of gained mixture is 15 ~ 25:1;
B, the mixture obtained by step a are placed in flash extracter and carry out homogenate extraction, obtain extracting solution;
C, step b gained extracting solution is carried out centrifugal, obtain supernatant liquor;
D, centrifugal rear remaining residue carry out extracting according to step b, c method again, centrifugal, obtain second time supernatant liquor, merge twice gained supernatant liquor;
E, adopt flash thickener to concentrate steps d gained supernatant liquor, obtain concentrated solution;
Adding 95% ethanol to system alcohol concn in the concentrated solution that f, step e obtain is 60 ~ 80%, carries out alcohol precipitation, is precipitated thing after standing, centrifugal;
G, the throw out distilled water obtained to be dissolved, being mixed with mass concentration is 10 ~ 50mg/mL solution, by Sevage ordinary method deproteination matter, Rabdosia rubescens polysaccharide soln after deproteination matter takes flash thickener to concentrate, gained concentrated solution, through vacuum lyophilization, obtains Rabdosia rubescens Crude polysaccharides;
H, step g gained Rabdosia rubescens Crude polysaccharides is added distilled water be mixed with Crude polysaccharides solution, then adopt DEAE-Celluose gel chromatographic columns to be separated, the liquid collecting main chromatographic peak carries out freeze-drying; Solid after obtained freeze-drying is adopted the NH of 0.05mol/L
4hCO
3solubilize, gained solution adopts Sephadex G200 gel chromatographic columns to be again separated, and collects main chromatographic peak liquid and carries out freeze-drying, obtain refining Rabdosia rubescens polysaccharide solid after freeze-drying.
2. the homogenate extraction method of Rabdosia rubescens polysaccharide according to claim 1, is characterized in that, extraction conditions when extracting in step b is: Extracting temperature is 50 ~ 70 DEG C, under 15000 ~ 20000 turns/min, extract 2 ~ 3min.
3. the homogenate extraction method of Rabdosia rubescens polysaccharide according to claim 1, is characterized in that, condition time centrifugal in step c, f is: at 4 DEG C, centrifugal 8 ~ 10min under 8000 ~ 10000 turns/min condition.
4. the homogenate extraction method of Rabdosia rubescens polysaccharide according to claim 1, is characterized in that, condition time concentrated in step e, g is: vacuum tightness be 0.08 ~ 0.098MPa, under temperature is the condition of 70 ~ 80 DEG C, concentrated 20 ~ 25s.
5. the homogenate extraction method of Rabdosia rubescens polysaccharide according to claim 1, is characterized in that: the condition left standstill in step f is leave standstill 24h under 4 DEG C of conditions.
6. the extracting and purifying method of Rabdosia rubescens polysaccharide according to claim 1, is characterized in that: the specification of DEAE-Celluose gel chromatographic columns is 5.0 × 50cm; When adopting DEAE-Celluose gel chromatographic columns to be separated, with the NaCl solution of 0.5mol/L for moving phase, flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method;
The specification of Sephadex G200 gel chromatographic columns is 5.0 × 50cm, when adopting Sephadex G200 gel chromatographic columns to be separated, with the NH of 0.05mol/L
4hCO
3solution is moving phase, and flow velocity is 2.0mL/min, develops the color to chromatographic solution with Phenol-sulphate acid method.
7. the application of Rabdosia rubescens polysaccharide in cigarette utilizing method described in claim 1 to extract.
8. the application of Rabdosia rubescens polysaccharide according to claim 7 in cigarette, is characterized in that: consumption when Rabdosia rubescens polysaccharide is applied in cigarette accounts for 0.005 ~ 0.1% of tobacco quality.
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