CN105061620A - Extraction and purification method for Trollius chinensis polysaccharide and application thereof as tobacco humectant - Google Patents
Extraction and purification method for Trollius chinensis polysaccharide and application thereof as tobacco humectant Download PDFInfo
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Abstract
The invention discloses an extraction and purification method for Trollius chinensis polysaccharide and application thereof as a tobacco humectant. The method includes: firstly drying and crushing Trollius chinensis, adding water into the crushed Trollius chinensis powder to perform soaking; then adding an enzyme preparation to conduct enzymolysis treatment, performing ultrasonic extraction after enzymolysis, subjecting the extracted solution to centrifugal separation, and carrying out pressure reduced concentration on the obtained supernate, adding ethanol to perform alcohol precipitation standing to obtain precipitate, i.e. Trollius chinensis crude polysaccharide; preparing the crude polysaccharide into a solution, removing protein by a polyamide column, subjecting the obtained solution to concentration and alcohol precipitation, and carrying out freeze drying on the obtained precipitate, thus obtaining refined Trollius chinensis polysaccharide. The Trollius chinensis polysaccharide extracted by the method provided by the invention has high purity, and the obtained Trollius chinensis polysaccharide can be dissolved to serve as a humectants to be applied in cigarettes, can achieve good physical and sensory moisturizing effect, also can reduce the irritation and miscellaneous gas of cigarettes, and improve the mellow sense and comfortableness of cigarettes.
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 extracting and purifying method of Flower of Chinese Globeflower polysaccharide and the application as tobacco humectant thereof.
Background technology
Usually need to add humectant to improve 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, thus 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.
At present, the polyhydroxy substances such as glycerine, propylene glycol, sorbyl alcohol are mainly adopted to be humectant in China's 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.
Polysaccharide 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 has stronger water-holding power.
Flower of Chinese Globeflower, as a kind of Chinese medicinal materials of dietotherapeutic, is the dried floral of ranunculaceae plant Flower of Chinese Globeflower.The non-product of wild resource enriches, and main product is in the Hebei of China, Shanxi, the Inner Mongol.Main chemical compositions has flavones, alkaloid, organic acid, volatilization wet goods.Mainly concentrate on anti-microbial activity, anti-inflammatory, anti-oxidant, anticancer and tea drink aspect to the research of Flower of Chinese Globeflower at present, the research in tobacco humectant has no pertinent literature report substantially.
Polysaccharide is one of main active substances of Flower of Chinese Globeflower, about extraction bibliographical information few of Flower of Chinese Globeflower polysaccharide, current bibliographical information has water-boiling method to extract polysaccharide, but there is operating time long, the defect such as temperature is high, yield is lower in water-boiling method, and the Crude polysaccharides extracted also has protein, protein in Crude polysaccharides has and strengthens flue gas and to mix the effect of gas, and therefore polysaccharide is applied on cigarette as humectant and needs deproteination matter in advance.
Summary of the invention
The technical problem to be solved in the present invention is: the defect not satisfactory according to humectant used in the deficiency of existing Flower of Chinese Globeflower polysaccharide extracting process and cigarette, the invention provides a kind of extracting and purifying method of Flower of Chinese Globeflower polysaccharide and the application as tobacco humectant thereof.The Flower of Chinese Globeflower purity of polysaccharide utilizing technical solution of the present invention to extract is high, is used in cigarette, has good physics and sense organ humectation effect, and can reduce the pungency of cigarette and assorted gas after being dissolved by gained Flower of Chinese Globeflower polysaccharide, improves mellow and full sense and the comfortableness of cigarette.
In order to solve the problem, the technical scheme that the present invention takes is:
The invention provides a kind of extracting and purifying method of Flower of Chinese Globeflower polysaccharide, described extracting and purifying method comprises the following steps:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen;
B, immersion: in the lily feet pollen obtained by step a, add water, the mass ratio that both lily feet pollen and water add is 1:20 ~ 25, then soaks 2 ~ 4h at ambient temperature;
C, ferment treatment: add zymin in the Flower of Chinese Globeflower solution after step b soaks and carry out enzymolysis processing, the add-on of zymin accounts for 0.5 ~ 3% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 60 ~ 80 DEG C, and ultrasonic extraction power is 300 ~ 500W, and ultrasonic time is 10 ~ 20min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 30 ~ 40% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 60 ~ 80%, leaves standstill 20 ~ 24h, carry out centrifugal after leaving standstill alcohol precipitation after adding ethanol, is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides that obtained by step f adopt polyamide column deproteination matter, and gained Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f again, alcohol precipitation, and then leave standstill centrifugal being precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide.
According to the extracting and purifying method of above-mentioned Flower of Chinese Globeflower polysaccharide, zymin described in step c is cellulase, and during enzymolysis processing, hydrolysis temperature is 35 ~ 54 DEG C, and enzymolysis time is 1 ~ 2h.
According to the extracting and purifying method of above-mentioned Flower of Chinese Globeflower polysaccharide, the condition in step e during centrifugation be 2 ~ 6 DEG C, under 8000 ~ 10000 turns/min, centrifugation time is 10 ~ 15min.
According to the extracting and purifying method of above-mentioned Flower of Chinese Globeflower polysaccharide, condition time centrifugal in step f be 2 ~ 6 DEG C, under 8000 ~ 10000 turns/min, centrifugation time is 10 ~ 15min.
According to the extracting and purifying method of above-mentioned Flower of Chinese Globeflower polysaccharide, the Crude polysaccharides obtained by step f described in step g adopts polyamide column deproteination matter, specific operation process is: the water first adding 1:3 ~ 6 times quality in Flower of Chinese Globeflower Crude polysaccharides, obtain Crude polysaccharides solution, then by the gained Crude polysaccharides aqueous solution through polyamide column, with water, wash-out is carried out to the polyamide column after absorption, by the protein that adsorbs not by wash-out, and by the Flower of Chinese Globeflower glycocalix water elution adsorbed, obtain Flower of Chinese Globeflower polysaccharide soln.
A kind of Flower of Chinese Globeflower polysaccharide utilizing aforesaid method to extract is as the application of tobacco humectant.
According to the application of above-mentioned Flower of Chinese Globeflower polysaccharide as tobacco humectant, consumption when Flower of Chinese Globeflower polysaccharide is applied in cigarette accounts for 0.005 ~ 0.1% of tobacco quality.
Flower of Chinese Globeflower polysaccharide is as humectant in cigarette application, and addition manner is evenly be sprayed onto in pipe tobacco after dilute with water, and polysaccharide add-on accounts for 0.005 ~ 0.1% of tobacco quality.
positive beneficial effect of the present invention:
1, extracting and purifying method of the present invention obtains the fine gold lotus flower polysaccharide of higher degree, during application by Flower of Chinese Globeflower polysaccharide after water dissolution, be sprayed on pipe tobacco by spray pattern, and the test of physics humid keeping performance and sensory quality assessment are carried out to it, find that it has good physics and sense organ humectation effect to cigarette, and the pungency of cigarette and assorted gas can be reduced, improve mellow and full sense and the comfortableness of cigarette.Therefore, the Flower of Chinese Globeflower polysaccharide of extraction purification of the present invention can be applied in cigarette as a kind of tobacco humectant of excellent property, and the Optimum of fine gold lotus flower polysaccharide in cigarette that the present invention extracts accounts for 0.005 ~ 0.1% of tobacco quality.
2, compared with prior art, the present invention mainly has the following advantages:
(1) adopt water logging-enzymolysis-ultrasonic-leaching method, make the extraction of Flower of Chinese Globeflower polysaccharide comparatively complete;
(2) adopt polyamide column adsorption-desorption method deproteinization, obtain the polysaccharide of higher degree, whole leaching process mild condition, raw material and the reagent of use are cheap and easy to get, simple to operate, and are convenient to fairly large production;
(3) prove through experiment, Flower of Chinese Globeflower polysaccharide of the present invention is to the humectation successful of tobacco product;
(4) the Flower of Chinese Globeflower polysaccharide prepared of the present invention, is applied on cigarette, does not change the original complete processing of cigarette, has more actual using value and meaning.
the polysaccharide content of inventive samples calculates:
the drafting of typical curve:
Accurately take 2.5000g dextrose anhydrous (analytical pure, 105 DEG C, baking oven is dried to constant weight) and be placed in 100mL volumetric flask, adding distil water constant volume, shakes up, and obtains glucose solution; The above-mentioned glucose solution of accurate measuring 1mL is placed in 50mL volumetric flask, with distilled water constant volume, obtains Glucose standards solution; Measure respectively 0.1,0.2,0.3,0.4,0.5 and 0.6mL Glucose standards solution be placed in tool plug test tube, respectively with water mend to 2mL, blank cuvette adds 2mL distilled water; In above test tube, respectively add 1mL distilled water, 6% phenol and the 5mL vitriol oil, shake up, room temperature places 20min, 30 DEG C of water-bath 25min, measures absorbancy with spectrophotometer at 490nm place.Take glucose content as X-coordinate, absorbance is ordinate zou drawing standard curve (refer to accompanying drawing 1 shown in).The regression equation of typical curve is: y=2.8839x-0.0015, coefficient R
2=0.9991, there is good linear relationship (referring to accompanying drawing 1).
polysaccharide content calculates:
Get Flower of Chinese Globeflower polysaccharide sample adding distil water to dissolve, be settled to 500mL; Get 1mL dilution again and be settled to 50mL; The above-mentioned sample solution of accurate measuring 1mL, adds 1mL distilled water, 1mL6% phenol and the 5mL vitriol oil, shakes up, and room temperature places 20min, 30 DEG C of water-bath 25min, measures absorbancy with spectrophotometer at 490nm place.Utilize typical curve can obtain the concentration of polysaccharide in Flower of Chinese Globeflower polysaccharide sample, calculate the content of polysaccharide further according to extension rate.
the mensuration of inventive samples moisturizing rate:take the Flower of Chinese Globeflower polysaccharide of preparation, 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) %.Timing measures the quality of polysaccharide solution, according to the moisturizing rate of this sample of mathematic interpolation.Meanwhile, compare with the distilled water of equivalent and same concentrations aqueous solution of propylene glycol.Flower of Chinese Globeflower polysaccharide, propylene glycol solution moisturizing rate under temperature (22 ± 1) DEG C, humidity (40 ± 2) % condition refers to table 1 over time.Result shows: relative to distilled water, propylene glycol control group, and Flower of Chinese Globeflower polysaccharide obviously can both slow down the speed of moisture loss at day part, significantly improves moisturizing rate.
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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 Flower of Chinese Globeflower polysaccharide prepared by the present invention, 5% aqueous solution is made into distilled water, evenly be sprayed onto (polysaccharide quality: tobacco quality=1:250) in equilibrated tobacco sample, 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, calculate the initial aqueous rate of each application of sample pipe tobacco after cooling.Often organize another 1 increment product, after precise, put into the climatic chamber that temperature is (22 ± 1) DEG C, humidity is (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: under (40%) condition that ambient relative humidity is lower, add Flower of Chinese Globeflower polysaccharide humectant, propylene glycol compared with blank pipe tobacco, moisture loss is relatively slower, and the moisture-retaining capacity of polysaccharide is better than propylene glycol, has good physics humid keeping performance.
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inventive samples sense organ humid keeping performance is tested:to make even the some parts of pure pipe tobacco after weighing apparatus [temperature be (22 ± 1) DEG C, relative humidity be (60% ± 2%), 48h], take Flower of Chinese Globeflower polysaccharide according to account for tobacco quality 0,0.01 ‰, 0.05 ‰, 0.10 ‰, 0.50 ‰, 1.0 ‰ and 2.0 ‰ respectively to add (the least possible) equivalent distilled water and be mixed with solution, spray equably with micro sprayer and be added on above-mentioned pipe tobacco.At temperature (40 ± 1) DEG C, 4h is 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 that cigarette puts into temperature (22 ± 1) DEG C with cigarette-roller, after relative humidity is the climatic chamber lower balance 48h of (60% ± 2%), smoke panel test; Smoking result refers to table 3.
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accompanying drawing illustrates:
Fig. 1 glucose standard curve.
embodiment:
Set forth the present invention further below in conjunction with embodiment, but do not limit content of the present invention.
Embodiment 1:
The extracting and purifying method of Flower of Chinese Globeflower polysaccharide of the present invention, its detailed step is as follows:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen 100g;
B, immersion: the water adding 20 times amount in the lily feet pollen obtained by step a, the mass ratio namely added both lily feet pollen and water is 1:20, then soaks 2h at ambient temperature;
C, ferment treatment: the Flower of Chinese Globeflower solution after being soaked by step b is heated to 40 DEG C, and add cellulase and carry out enzymolysis processing 2h, the add-on of cellulase accounts for 1.5% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 60 DEG C, and ultrasonic extraction power is 300W, and ultrasonic time is 10min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation, 2 DEG C, under 8000 turns/min, centrifugal 15min;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 35% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 60%, leaves standstill 22h after adding ethanol, leaves standstill alcohol precipitation postprecipitation and goes out Flower of Chinese Globeflower polysaccharide, and then at 2 DEG C, under 8000 turns/min, centrifugal 15min is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides obtained by step f add water according to the mass ratio of 1:3 and dissolve in Crude polysaccharides, obtain Crude polysaccharides solution, then polyamide column deproteination matter is adopted, obtain that Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f, alcohol precipitation, leave standstill, to be centrifugally precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide 6.27g, yield 6.27%, polysaccharide content 27.86%.
Embodiment 2:
The extracting and purifying method of Flower of Chinese Globeflower polysaccharide of the present invention, its detailed step is as follows:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen 100g;
B, immersion: the water adding 22 times amount in the lily feet pollen obtained by step a, the mass ratio namely added both lily feet pollen and water is 1:22, then soaks 3h at ambient temperature;
C, ferment treatment: the Flower of Chinese Globeflower solution after being soaked by step b is heated to 45 DEG C, and add cellulase and carry out enzymolysis processing 1h, the add-on of cellulase accounts for 2.0% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 70 DEG C, and ultrasonic extraction power is 400W, and ultrasonic time is 13min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation, 4 DEG C, under 9000 turns/min, centrifugal 15min;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 30% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 70%, leaves standstill 24h after adding ethanol, leaves standstill alcohol precipitation postprecipitation and goes out Flower of Chinese Globeflower polysaccharide, and then at 4 DEG C, under 9000 turns/min, centrifugal 15min is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides obtained by step f add water according to the mass ratio of 1:4 and dissolve in Crude polysaccharides, obtain Crude polysaccharides solution, then polyamide column deproteination matter is adopted, obtain that Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f, alcohol precipitation, leave standstill, to be centrifugally precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide 7.13g, yield 7.13%, polysaccharide content 28.55%.
Embodiment 3:
The extracting and purifying method of Flower of Chinese Globeflower polysaccharide of the present invention, its detailed step is as follows:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen 100g;
B, immersion: the water adding 25 times amount in the lily feet pollen obtained by step a, the mass ratio namely added both lily feet pollen and water is 1:25, then soaks 4h at ambient temperature;
C, ferment treatment: the Flower of Chinese Globeflower solution after being soaked by step b is heated to 54 DEG C, and add cellulase and carry out enzymolysis processing 1h, the add-on of cellulase accounts for 2.5% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 80 DEG C, and ultrasonic extraction power is 500W, and ultrasonic time is 10min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation, 6 DEG C, under 10000 turns/min, centrifugal 10min;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 40% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 80%, leaves standstill 22h after adding ethanol, leaves standstill alcohol precipitation postprecipitation and goes out Flower of Chinese Globeflower polysaccharide, and then at 6 DEG C, under 10000 turns/min, centrifugal 10min is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides obtained by step f add water according to the mass ratio of 1:4 and dissolve in Crude polysaccharides, obtain Crude polysaccharides solution, then polyamide column deproteination matter is adopted, obtain that Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f, alcohol precipitation, leave standstill, to be centrifugally precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide 6.31g, yield 6.31%, polysaccharide content 28.39%.
Embodiment 4:
The extracting and purifying method of Flower of Chinese Globeflower polysaccharide of the present invention, its detailed step is as follows:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen 100g;
B, immersion: the water adding 22 times amount in the lily feet pollen obtained by step a, the mass ratio namely added both lily feet pollen and water is 1:22, then soaks 3h at ambient temperature;
C, ferment treatment: the Flower of Chinese Globeflower solution after being soaked by step b is heated to 35 DEG C, and add cellulase and carry out enzymolysis processing 1h, the add-on of cellulase accounts for 1.0% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 65 DEG C, and ultrasonic extraction power is 350W, and ultrasonic time is 16min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation, 2 DEG C, under 10000 turns/min, centrifugal 15min;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 40% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 65%, leaves standstill 20h after adding ethanol, leaves standstill alcohol precipitation postprecipitation and goes out Flower of Chinese Globeflower polysaccharide, and then at 2 DEG C, under 10000 turns/min, centrifugal 15min is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides obtained by step f add water according to the mass ratio of 1:5 and dissolve in Crude polysaccharides, obtain Crude polysaccharides solution, then polyamide column deproteination matter is adopted, obtain that Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f, alcohol precipitation, leave standstill, to be centrifugally precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide 6.47g, polysaccharide yield 6.47%, polysaccharide content 27.05%.
Embodiment 5:
The extracting and purifying method of Flower of Chinese Globeflower polysaccharide of the present invention, its detailed step is as follows:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen 100g;
B, immersion: the water adding 20 times amount in the lily feet pollen obtained by step a, the mass ratio namely added both lily feet pollen and water is 1:20, then soaks 2h at ambient temperature;
C, ferment treatment: the Flower of Chinese Globeflower solution after being soaked by step b is heated to 50 DEG C, and add cellulase and carry out enzymolysis processing 1.5h, the add-on of cellulase accounts for 2.0% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 75 DEG C, and ultrasonic extraction power is 300W, and ultrasonic time is 12min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation, 4 DEG C, under 8000 turns/min, centrifugal 13min;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 40% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 75%, leaves standstill 24h after adding ethanol, leaves standstill alcohol precipitation postprecipitation and goes out Flower of Chinese Globeflower polysaccharide, and then at 4 DEG C, under 8000 turns/min, centrifugal 13min is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides obtained by step f add water according to the mass ratio of 1:6 and dissolve in Crude polysaccharides, obtain Crude polysaccharides solution, then polyamide column deproteination matter is adopted, obtain that Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f, alcohol precipitation, leave standstill, to be centrifugally precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide 6.48g, polysaccharide yield 6.48%, polysaccharide content 28.29%.
Embodiment 6:
Take according to the ratio accounting for tobacco quality 0.001% the fine gold lotus flower polysaccharide that embodiment 1 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking 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 fine gold lotus flower polysaccharide that embodiment 1 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity slightly increases, and flue gas is slightly soft, slightly returns sweet sense, and stimulate slightly little, comfortable taste slightly increases (referring to table 3).
Embodiment 8:
Take according to the ratio accounting for tobacco quality 0.01% the fine gold lotus flower polysaccharide that embodiment 1 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity slightly increases, and flue gas slightly 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 fine gold lotus flower polysaccharide that embodiment 1 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity slightly increases, and 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 fine gold lotus flower polysaccharide that embodiment 1 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity increases, and flue gas obviously becomes mellow and full, soft, and return sweet sense obviously, comfortable taste promotes, assorted gas and pungency low (referring to table 3).
Embodiment 11:
Take according to the ratio accounting for tobacco quality 0.2% the fine gold lotus flower polysaccharide that embodiment 1 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity increases, and pungency strengthens, and pleasant impression is slightly deteriorated (referring to table 3).
Embodiment 12:
Take according to the ratio accounting for tobacco quality 0.05% the fine gold lotus flower polysaccharide that embodiment 2 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity slightly increases, and flue gas obviously becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste promotes, and assorted gas and pungency reduce.
Embodiment 13:
Take according to the ratio accounting for tobacco quality 0.1% the fine gold lotus flower polysaccharide that embodiment 3 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity increases, and flue gas obviously becomes mellow and full, soft, and it is obvious to return sweet sense, and comfortable taste promotes, assorted gas and pungency low.
Embodiment 14:
Take according to the ratio accounting for tobacco quality 0.01% the fine gold lotus flower polysaccharide that embodiment 4 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity slightly increases, and flue gas slightly becomes mellow and full, soft, and return sweet sense and strengthen, comfortable taste slightly increases, and assorted gas and pungency slightly reduce.
Embodiment 15:
Take according to the ratio accounting for tobacco quality 0.005% the fine gold lotus flower polysaccharide that embodiment 5 obtains, add distilled water and be mixed with solution, Flower of Chinese Globeflower polysaccharide soln is evenly sprayed onto on pipe tobacco, roll into cigarette after baking and smoke panel test.Smoking result shows, perfume quantity slightly increases, and flue gas is slightly soft, slightly returns sweet sense, and stimulate slightly little, comfortable taste slightly increases.
Claims (7)
1. an extracting and purifying method for Flower of Chinese Globeflower polysaccharide, is characterized in that, described extracting and purifying method comprises the following steps:
A, drying and crushing: Flower of Chinese Globeflower crushed after being dried is become 40 ~ 60 object powder, obtain lily feet pollen;
B, immersion: in the lily feet pollen obtained by step a, add water, the mass ratio that both lily feet pollen and water add is 1:20 ~ 25, then soaks 2 ~ 4h at ambient temperature;
C, ferment treatment: add zymin in the Flower of Chinese Globeflower solution after step b soaks and carry out enzymolysis processing, the add-on of zymin accounts for 0.5 ~ 3% of Flower of Chinese Globeflower opaque amount;
D, supersound extraction: the Flower of Chinese Globeflower solution after step c enzymolysis is carried out ultrasonic extraction, Extracting temperature is 60 ~ 80 DEG C, and ultrasonic extraction power is 300 ~ 500W, and ultrasonic time is 10 ~ 20min;
E, solid-liquid separation: the extracting solution after steps d supersound extraction is carried out centrifugation;
F, concentrated alcohol precipitation: centrifugal for step e rear gained supernatant liquor is carried out concentrating under reduced pressure, is concentrated into 30 ~ 40% of former supernatant volume; Then adding 95% ethanol to system alcohol concn is 60 ~ 80%, leaves standstill 20 ~ 24h, carry out centrifugal after leaving standstill alcohol precipitation after adding ethanol, is precipitated i.e. Flower of Chinese Globeflower Crude polysaccharides;
G, the Flower of Chinese Globeflower Crude polysaccharides that obtained by step f adopt polyamide column deproteination matter, and gained Flower of Chinese Globeflower polysaccharide soln carries out concentrating according to step f again, alcohol precipitation, and then leave standstill centrifugal being precipitated, gained precipitation, through lyophilize, obtains fine gold lotus flower polysaccharide.
2. the extracting and purifying method of Flower of Chinese Globeflower polysaccharide according to claim 1, it is characterized in that: zymin described in step c is cellulase, during enzymolysis processing, hydrolysis temperature is 35 ~ 54 DEG C, enzymolysis time is 1 ~ 2h.
3. the extracting and purifying method of Flower of Chinese Globeflower polysaccharide according to claim 1, is characterized in that: the condition in step e during centrifugation for 2 ~ 6 DEG C, under 8000 ~ 10000 turns/min, centrifugation time is 10 ~ 15min.
4. the extracting and purifying method of Flower of Chinese Globeflower polysaccharide according to claim 1, is characterized in that: condition time centrifugal in step f for 2 ~ 6 DEG C, under 8000 ~ 10000 turns/min, centrifugation time is 10 ~ 15min.
5. the extracting and purifying method of Flower of Chinese Globeflower polysaccharide according to claim 1, it is characterized in that, the Crude polysaccharides obtained by step f described in step g adopts polyamide column deproteination matter, specific operation process is: the water first adding 1:3 ~ 6 times quality in Flower of Chinese Globeflower Crude polysaccharides, obtain Crude polysaccharides solution, then by the gained Crude polysaccharides aqueous solution through polyamide column, with water, wash-out is carried out to the polyamide column after absorption, by the protein that adsorbs not by wash-out, and by the Flower of Chinese Globeflower glycocalix water elution adsorbed, obtain Flower of Chinese Globeflower polysaccharide soln.
6. one kind utilizes the application of Flower of Chinese Globeflower polysaccharide as tobacco humectant of method extraction described in claim 1.
7. Flower of Chinese Globeflower polysaccharide according to claim 6 is as the application of tobacco humectant, it is characterized in that: consumption when Flower of Chinese Globeflower polysaccharide is applied in cigarette accounts for 0.005 ~ 0.1% of tobacco quality.
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| CN114904016A (en) * | 2022-04-14 | 2022-08-16 | 华南理工大学 | Clathrate compound containing trollius chinensis bunge extract and preparation method and application thereof |
| CN114904016B (en) * | 2022-04-14 | 2023-12-19 | 华南理工大学 | Clathrate containing trollius chinensis bunge extract and preparation method and application thereof |
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