CN105601948B - A kind of method that plantago asiatica linne polyoses viscosity is reduced using tea polyphenols - Google Patents
A kind of method that plantago asiatica linne polyoses viscosity is reduced using tea polyphenols Download PDFInfo
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Abstract
A kind of method that plantago asiatica linne polyoses viscosity is reduced using tea polyphenols,（1）A certain amount of dry plantain seed is weighed, water-soluble plantago asiatica linne polyoses are prepared using hot water extraction, ethanol precipitation, remaining plantain seed residue is extracted with NaOH again, and extracting solution is concentrated, alcohol precipitation, Sevag methods take off albumen, obtains alkali solubility plantago asiatica linne polyoses；Or with after the low stickiness component of warm water extraction, residue uses boiling waterbath again, then obtains plantago asiatica linne polyoses by concentration, alcohol precipitation, de- albumen；（2）Above-mentioned plantago asiatica linne polyoses are weighed respectively, are 1 according to plantago asiatica linne polyoses and aqueous solution mass volume ratio:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025 ~ 0.2%, and plantago asiatica linne polyoses are uniformly mixed with tea polyphenols respectively, obtain low-viscosity plantago asiatica linne polyoses solution.The present invention can significantly reduce plantago asiatica linne polyoses solution viscosity after adding a small amount of tea polyphenols；The plantago asiatica linne polyoses being prepared suitable for various extracting methods.
Description
Technical field
The invention belongs to natural products preparation field.
Background technology
Plantain seed is plantago plant Chinese herbaceous peonyPlantago asiaticaOr ordinary building L.Plantago derpressa
Willd. dry mature seed, when summer, two season of autumn seed maturity, harvest fruit ear, rub seed, remove impurity and obtain, by China
Food and medicine Surveillance Authority is classified as the article available for health food." plantain seed is sweet in flavor cold nontoxic；The main infirmity analgesic of gas, Li Shui
Diuresis, except arthritis with fixed pain caused by dampness；Long term usage is made light of one's life by commiting suicide resistance to old ", it is that China's ancient times are earliest and one of the most widely used certified products medicinal material.
The main polysaccharide extracted from plantain seed, is a kind of component rich in araboxylan, and viscosity is very high, when
Polysaccharide concentration is somewhat higher just to form Weak Gels.Modern research shows that plantago asiatica linne polyoses have many functional activities, including it is anti-
Oxygen, hypoglycemic, reducing blood lipid and adjusting body's immunity etc., while plantago asiatica linne polyoses high viscosity feature, assign its ease constipation and lead to
Just, promote the physiological functions such as intestinal health, increase excrement water content, and can play and remove the special works such as internal heavy metal
With.But high viscosity feature also adds inconvenience for its production and application, particularly to after drying polyose plus water answer
Dissolubility produces considerable influence, while can increase plantago asiatica linne polyoses production, the energy consumption in preparation process, this problem all the time by
To people's common concern but make slow progress.Therefore, it is necessary to by certain technology and method, effectively reduce plantago asiatica linne polyoses and stick
Degree, while ensure low cost, promote the further of plantago asiatica linne polyoses to develop and use with this, increase economic benefit.
The content of the invention
It is an object of the invention to provide one kind plantago asiatica linne polyoses are reduced using tea polyphenols（Plantago asiatica L.
Crude Polysaccharide, PLCP）The method of viscosity.
The present invention is achieved by the following technical solutions.
The present invention is according to the following steps.
（1）It is prepared by plantago asiatica linne polyoses：A certain amount of dry plantain seed is weighed, water is prepared using hot water extraction, ethanol precipitation
Dissolubility plantago asiatica linne polyoses, remaining plantain seed residue are extracted with NaOH again, and extracting solution is concentrated, alcohol precipitation, Sevag methods take off the step such as albumen
Suddenly, alkali solubility plantago asiatica linne polyoses are obtained.
（2）It is prepared by low viscosity plantago asiatica linne polyoses：A certain amount of above-mentioned water-soluble plantago asiatica linne polyoses or alkali solubility are weighed respectively
Plantago asiatica linne polyoses, according to plantago asiatica linne polyoses and aqueous solution mass volume ratio（g/L）For 1:5 ratio dissolving polysaccharide, it is more to add tea
Phenol, the mass fraction of tea polyphenols is 0.025 ~ 0.2%, respectively by water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses and tea
Polyphenol after mixing, obtains low-viscosity plantago asiatica linne polyoses solution.
The present invention can also be according to the following steps.
（1）A certain amount of dry plantain seed is weighed, after extracting low stickiness component with warm water, residue uses boiling waterbath again, so
Afterwards by concentration, alcohol precipitation, de- albumen and etc. obtain plantago asiatica linne polyoses.
（2）A certain amount of above-mentioned plantago asiatica linne polyoses are weighed, according to plantago asiatica linne polyoses and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025 ~ 0.2%, by above-mentioned polysaccharide and tea polyphenols
It is uniformly mixed, obtains low-viscosity plantago asiatica linne polyoses solution.
The plantago asiatica linne polyoses that plantago asiatica linne polyoses of the present invention can also be commercially available or prepared by the extraction of other methods.
It is an advantage of the invention that：1st, plantago asiatica linne polyoses solution viscosity can be significantly reduced after adding a small amount of tea polyphenols；2nd, fit
The plantago asiatica linne polyoses being prepared for various extracting methods；3rd, a small amount of tea polyphenols are added to be uniformly mixed with plantago asiatica linne polyoses solution
After drying, remain to effectively reduce polysaccharide solution viscosity, add the effect that water redissolves better than undressed polysaccharide as former state.
Brief description of the drawings
Fig. 1 is influence of the different tea polyphenols additive amounts to plantago asiatica linne polyoses PLCP-1 apparent viscosities.
Fig. 2 is influence of the different tea polyphenols additive amounts to plantago asiatica linne polyoses PLCP-2 apparent viscosities.
Fig. 3 is influence of the different tea polyphenols additive amounts to plantago asiatica linne polyoses PLCP-3 apparent viscosities.
Fig. 4 is influence of the different tea polyphenols additive amounts to plantago asiatica linne polyoses PLCP-1 apparent viscosities（Polysaccharide adds tea polyphenols
First it is freeze-dried afterwards, then adds water redissolution test）.
Fig. 5 is influence of the different tea polyphenols additive amounts to plantago asiatica linne polyoses PLCP-2 apparent viscosities（Polysaccharide adds tea polyphenols
First it is freeze-dried afterwards, then adds water redissolution test）.
Fig. 6 is influence of the different tea polyphenols additive amounts to plantago asiatica linne polyoses PLCP-3 apparent viscosities（Polysaccharide adds tea polyphenols
First it is freeze-dried afterwards, then adds water redissolution test）.
Embodiment
Technical scheme is clearly and completely described below by embodiment, described embodiment is only
Only it is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those skilled in the art
The other embodiment obtained without making creative work, belongs to the scope of protection of the invention.
Embodiment 1.
Weigh a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, 24 h of immersion with
On, plantain seed is collected by filtration, is placed in baking oven dry.Then the above-mentioned plantain seeds of 100 g are weighed and carry out water-bath extraction, extraction
Temperature is 100oC, the mass volume ratio of feed liquid（kg/L）For 1:10, extract 2 times, each extraction time is 3 h, with rotating speed 4800
R/min, 10 min of time centrifuge extracting solution and plantain seed；Merge the supernatant extracted twice, add after vacuum concentration
Enter the ethanol precipitation that mass fraction is 95%, final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；Rotating speed 4800
Precipitation is collected by centrifugation in r/min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gained
Component obtains water-soluble plantago asiatica linne polyoses PLCP-1 after freeze-drying again.Plantain seed after above-mentioned steps are extracted is residual
Slag is dried, then the mass volume ratio of alkali-soluble polysaccharide component, plantain seed and NaOH solution is extracted with NaOH solution（kg/L）For 1:
10,4 DEG C of Extracting temperature, 2 h of extraction time, is extracted 2 times, each extraction time is 3 h, with 4800 r/min of rotating speed, time 10
Min centrifuges extracting solution and plantain seed, adds acetic acid neutralization；Merge the supernatant for extracting, being obtained after neutralization twice, vacuum
Mass fraction is added after concentration as 95% ethanol precipitation, final ethanol mass fraction is 80% in system, is refrigerated at 4 DEG C
Night；Precipitation is collected by centrifugation in 4800 r/min of rotating speed, 10 min of time, is redissolved again in water after freeze-drying, anti-using Sevag methods
Albumen is taken off again, is collected polysaccharide solution and is dialysed；Dialyzate is concentrated in vacuo after dialysis, then toward adding quality in concentrate
Fraction is 95% ethanol precipitation, and final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；4800 r/ of rotating speed
Precipitation is collected by centrifugation in min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gains
Matter obtains alkali solubility plantago asiatica linne polyoses PLCP-2 by freeze-drying again.
10 g plantago asiatica linne polyoses PLCP-1, PLCP-2 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025%, can significantly reduce plantago asiatica linne polyoses and stick
Degree.
Embodiment 2.
Plantain seed is placed in the ethanol that mass fraction is 80% and soaks 12 more than h, for several times, then filtering is received for during which stirring
Collect plantain seed, be placed in drying box dry；Plantain seed is after removal of impurities, by plantain seed and the mass volume ratio of water（kg/L）For 1:10
Ratio, 50oC warm water extracts, and extraction time 2 times, each 3 h of extraction time, is filtered after extraction, collects plantain seed；Car
Preceding son continues on for follow-up water-bath extraction, Extracting temperature 100oThe quality volume of C, plantain seed and water（kg/L）Than for 1:10,
Extraction time 2 times, each 3 h of extraction time；Extracting solution is centrifuged, and centrifugal rotational speed is controlled in 4800 r/min, centrifugation time
10 min, collect supernatant polysaccharide solution and are concentrated；The ethanol that mass fraction is 95% is added into concentrate to be precipitated,
The final concentration of mass fraction 80% of final ethanol in system, stands 12 more than h and precipitation is collected by centrifugation again, precipitation plus water are answered
It is molten, albumen is taken off using Sevag methods repeatedly, polysaccharide solution is collected and dialyses；Dialyzate is concentrated in vacuo after dialysis, is cold
It is lyophilized dry, obtain plantago asiatica linne polyoses PLCP-3.
10 g plantago asiatica linne polyoses PLCP-3 are weighed, according to raw material and aqueous solution mass volume ratio（g/L）For 1:5 ratio is molten
Polysaccharide is solved, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 3.
Weigh a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, 24 h of immersion with
On, plantain seed is collected by filtration, is placed in baking oven dry.Then the above-mentioned plantain seeds of 100 g are weighed and carry out water-bath extraction, extraction
Temperature is 100oC, the mass volume ratio of feed liquid（kg/L）For 1:10, extract 2 times, each extraction time is 3 h, with rotating speed 4800
R/min, 10 min of time centrifuge extracting solution and plantain seed；Merge the supernatant extracted twice, add after vacuum concentration
Enter the ethanol precipitation that mass fraction is 95%, final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；Rotating speed 4800
Precipitation is collected by centrifugation in r/min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gained
Component obtains water-soluble plantago asiatica linne polyoses PLCP-1 after freeze-drying again.Plantain seed after above-mentioned steps are extracted is residual
Slag is dried, then the mass volume ratio of alkali-soluble polysaccharide component, plantain seed and NaOH solution is extracted with NaOH solution（kg/L）For 1:
10,4 DEG C of Extracting temperature, 2 h of extraction time, is extracted 2 times, each extraction time is 3 h, with 4800 r/min of rotating speed, time 10
Min centrifuges extracting solution and plantain seed, adds acetic acid neutralization；Merge the supernatant for extracting, being obtained after neutralization twice, vacuum
Mass fraction is added after concentration as 95% ethanol precipitation, final ethanol mass fraction is 80% in system, is refrigerated at 4 DEG C
Night；Precipitation is collected by centrifugation in 4800 r/min of rotating speed, 10 min of time, is redissolved again in water after freeze-drying, anti-using Sevag methods
Albumen is taken off again, is collected polysaccharide solution and is dialysed；Dialyzate is concentrated in vacuo after dialysis, then toward adding quality in concentrate
Fraction is 95% ethanol precipitation, and final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；4800 r/ of rotating speed
Precipitation is collected by centrifugation in min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gains
Matter obtains alkali solubility plantago asiatica linne polyoses PLCP-2 by freeze-drying again.
10 g plantago asiatica linne polyoses PLCP-1, PLCP-2 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.05%, can significantly reduce plantago asiatica linne polyoses and stick
Degree.
Embodiment 4.
Plantain seed is placed in the ethanol that mass fraction is 80% and soaks 12 more than h, for several times, then filtering is received for during which stirring
Collect plantain seed, be placed in drying box dry；Plantain seed is after removal of impurities, by plantain seed and the mass volume ratio of water（kg/L）For 1:10
Ratio, 50oC warm water extracts, and extraction time 2 times, each 3 h of extraction time, is filtered after extraction, collects plantain seed；Car
Preceding son continues on for follow-up water-bath extraction, Extracting temperature 100oThe quality volume of C, plantain seed and water（kg/L）Than for 1:10,
Extraction time 2 times, each 3 h of extraction time；Extracting solution is centrifuged, and centrifugal rotational speed is controlled in 4800 r/min, centrifugation time
10 min, collect supernatant polysaccharide solution and are concentrated；The ethanol that mass fraction is 95% is added into concentrate to be precipitated,
The final concentration of mass fraction 80% of final ethanol in system, stands 12 more than h and precipitation is collected by centrifugation again, precipitation plus water are answered
It is molten, albumen is taken off using Sevag methods repeatedly, polysaccharide solution is collected and dialyses；Dialyzate is concentrated in vacuo after dialysis, is cold
It is lyophilized dry, obtain plantago asiatica linne polyoses PLCP-3.
10 g plantago asiatica linne polyoses PLCP-3 are weighed, according to raw material and aqueous solution mass volume ratio（g/L）For 1:5 ratio is molten
Polysaccharide is solved, adds tea polyphenols, the mass fraction of tea polyphenols is 0.05%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 5.
Weigh a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, 24 h of immersion with
On, plantain seed is collected by filtration, is placed in baking oven dry.Then the above-mentioned plantain seeds of 100 g are weighed and carry out water-bath extraction, extraction
Temperature is 100oC, the mass volume ratio of feed liquid（kg/L）For 1:10, extract 2 times, each extraction time is 3 h, with rotating speed 4800
R/min, 10 min of time centrifuge extracting solution and plantain seed；Merge the supernatant extracted twice, add after vacuum concentration
Enter the ethanol precipitation that mass fraction is 95%, final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；Rotating speed 4800
Precipitation is collected by centrifugation in r/min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gained
Component obtains water-soluble plantago asiatica linne polyoses PLCP-1 after freeze-drying again.Plantain seed after above-mentioned steps are extracted is residual
Slag is dried, then the mass volume ratio of alkali-soluble polysaccharide component, plantain seed and NaOH solution is extracted with NaOH solution（kg/L）For 1:
10,4 DEG C of Extracting temperature, 2 h of extraction time, is extracted 2 times, each extraction time is 3 h, with 4800 r/min of rotating speed, time 10
Min centrifuges extracting solution and plantain seed, adds acetic acid neutralization；Merge the supernatant for extracting, being obtained after neutralization twice, vacuum
Mass fraction is added after concentration as 95% ethanol precipitation, final ethanol mass fraction is 80% in system, is refrigerated at 4 DEG C
Night；Precipitation is collected by centrifugation in 4800 r/min of rotating speed, 10 min of time, is redissolved again in water after freeze-drying, anti-using Sevag methods
Albumen is taken off again, is collected polysaccharide solution and is dialysed；Dialyzate is concentrated in vacuo after dialysis, then toward adding quality in concentrate
Fraction is 95% ethanol precipitation, and final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；4800 r/ of rotating speed
Precipitation is collected by centrifugation in min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gains
Matter obtains alkali solubility plantago asiatica linne polyoses PLCP-2 by freeze-drying again.
10 g plantago asiatica linne polyoses PLCP-1, PLCP-2 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.2%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 6.
Plantain seed is placed in the ethanol that mass fraction is 80% and soaks 12 more than h, for several times, then filtering is received for during which stirring
Collect plantain seed, be placed in drying box dry；Plantain seed is after removal of impurities, by plantain seed and the mass volume ratio of water（kg/L）For 1:10
Ratio, 50oC warm water extracts, and extraction time 2 times, each 3 h of extraction time, is filtered after extraction, collects plantain seed；Car
Preceding son continues on for follow-up water-bath extraction, Extracting temperature 100oThe quality volume of C, plantain seed and water（kg/L）Than for 1:10,
Extraction time 2 times, each 3 h of extraction time；Extracting solution is centrifuged, and centrifugal rotational speed is controlled in 4800 r/min, centrifugation time
10 min, collect supernatant polysaccharide solution and are concentrated；The ethanol that mass fraction is 95% is added into concentrate to be precipitated,
The final concentration of mass fraction 80% of final ethanol in system, stands 12 more than h and precipitation is collected by centrifugation again, precipitation plus water are answered
It is molten, albumen is taken off using Sevag methods repeatedly, polysaccharide solution is collected and dialyses；Dialyzate is concentrated in vacuo after dialysis, is cold
It is lyophilized dry, obtain plantago asiatica linne polyoses PLCP-3.
10 g plantago asiatica linne polyoses PLCP-3 are weighed, according to raw material and aqueous solution mass volume ratio（g/L）For 1:5 ratio is molten
Polysaccharide is solved, adds tea polyphenols, the mass fraction of tea polyphenols is 0.2%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 7.
Weigh a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, 24 h of immersion with
On, plantain seed is collected by filtration, is placed in baking oven dry.Then the above-mentioned plantain seeds of 100 g are weighed and carry out water-bath extraction, extraction
Temperature is 100oC, the mass volume ratio of feed liquid（kg/L）For 1:10, extract 2 times, each extraction time is 3 h, with rotating speed 4800
R/min, 10 min of time centrifuge extracting solution and plantain seed；Merge the supernatant extracted twice, add after vacuum concentration
Enter the ethanol precipitation that mass fraction is 95%, final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；Rotating speed 4800
Precipitation is collected by centrifugation in r/min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gained
Component obtains water-soluble plantago asiatica linne polyoses PLCP-1 after freeze-drying again.Plantain seed after above-mentioned steps are extracted is residual
Slag is dried, then the mass volume ratio of alkali-soluble polysaccharide component, plantain seed and NaOH solution is extracted with NaOH solution（kg/L）For 1:
10,4 DEG C of Extracting temperature, 2 h of extraction time, is extracted 2 times, each extraction time is 3 h, with 4800 r/min of rotating speed, time 10
Min centrifuges extracting solution and plantain seed, adds acetic acid neutralization；Merge the supernatant for extracting, being obtained after neutralization twice, vacuum
Mass fraction is added after concentration as 95% ethanol precipitation, final ethanol mass fraction is 80% in system, is refrigerated at 4 DEG C
Night；Precipitation is collected by centrifugation in 4800 r/min of rotating speed, 10 min of time, is redissolved again in water after freeze-drying, anti-using Sevag methods
Albumen is taken off again, is collected polysaccharide solution and is dialysed；Dialyzate is concentrated in vacuo after dialysis, then toward adding quality in concentrate
Fraction is 95% ethanol precipitation, and final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；4800 r/ of rotating speed
Precipitation is collected by centrifugation in min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gains
Matter obtains alkali solubility plantago asiatica linne polyoses PLCP-2 by freeze-drying again.
10 g plantago asiatica linne polyoses PLCP-1, PLCP-2 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025%, is then freeze-dried, gained car
Preceding sub- polysaccharide viscosity significantly reduces.
Embodiment 8.
Plantain seed is placed in the ethanol that mass fraction is 80% and soaks 12 more than h, for several times, then filtering is received for during which stirring
Collect plantain seed, be placed in drying box dry；Plantain seed is after removal of impurities, by plantain seed and the mass volume ratio of water（kg/L）For 1:10
Ratio, 50oC warm water extracts, and extraction time 2 times, each 3 h of extraction time, is filtered after extraction, collects plantain seed；Car
Preceding son continues on for follow-up water-bath extraction, Extracting temperature 100oThe quality volume of C, plantain seed and water（kg/L）Than for 1:10,
Extraction time 2 times, each 3 h of extraction time；Extracting solution is centrifuged, and centrifugal rotational speed is controlled in 4800 r/min, centrifugation time
10 min, collect supernatant polysaccharide solution and are concentrated；The ethanol that mass fraction is 95% is added into concentrate to be precipitated,
The final concentration of mass fraction 80% of final ethanol in system, stands 12 more than h and precipitation is collected by centrifugation again, precipitation plus water are answered
It is molten, albumen is taken off using Sevag methods repeatedly, polysaccharide solution is collected and dialyses；Dialyzate is concentrated in vacuo after dialysis, is cold
It is lyophilized dry, obtain plantago asiatica linne polyoses PLCP-3.
10 g plantago asiatica linne polyoses PLCP-3 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For 1:5 ratio
Example dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025%, is then freeze-dried, gained plantain seed is more
Sugared viscosity significantly reduces.
Embodiment 9.
Weigh a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, 24 h of immersion with
On, plantain seed is collected by filtration, is placed in baking oven dry.Then the above-mentioned plantain seeds of 100 g are weighed and carry out water-bath extraction, extraction
Temperature is 100oC, the mass volume ratio of feed liquid（kg/L）For 1:10, extract 2 times, each extraction time is 3 h, with rotating speed 4800
R/min, 10 min of time centrifuge extracting solution and plantain seed；Merge the supernatant extracted twice, add after vacuum concentration
Enter the ethanol precipitation that mass fraction is 95%, final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；Rotating speed 4800
Precipitation is collected by centrifugation in r/min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gained
Component obtains water-soluble plantago asiatica linne polyoses PLCP-1 after freeze-drying again.Plantain seed after above-mentioned steps are extracted is residual
Slag is dried, then the mass volume ratio of alkali-soluble polysaccharide component, plantain seed and NaOH solution is extracted with NaOH solution（kg/L）For 1:
10,4 DEG C of Extracting temperature, 2 h of extraction time, is extracted 2 times, each extraction time is 3 h, with 4800 r/min of rotating speed, time 10
Min centrifuges extracting solution and plantain seed, adds acetic acid neutralization；Merge the supernatant for extracting, being obtained after neutralization twice, vacuum
Mass fraction is added after concentration as 95% ethanol precipitation, final ethanol mass fraction is 80% in system, is refrigerated at 4 DEG C
Night；Precipitation is collected by centrifugation in 4800 r/min of rotating speed, 10 min of time, is redissolved again in water after freeze-drying, anti-using Sevag methods
Albumen is taken off again, is collected polysaccharide solution and is dialysed；Dialyzate is concentrated in vacuo after dialysis, then toward adding quality in concentrate
Fraction is 95% ethanol precipitation, and final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；4800 r/ of rotating speed
Precipitation is collected by centrifugation in min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gains
Matter obtains alkali solubility plantago asiatica linne polyoses PLCP-2 by freeze-drying again.
10 g plantago asiatica linne polyoses PLCP-1, PLCP-2 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.05%, is then freeze-dried, gained car
Preceding sub- polysaccharide viscosity significantly reduces.
Embodiment 10.
Plantain seed is placed in the ethanol that mass fraction is 80% and soaks 12 more than h, for several times, then filtering is received for during which stirring
Collect plantain seed, be placed in drying box dry；Plantain seed is after removal of impurities, by plantain seed and the mass volume ratio of water（kg/L）For 1:10
Ratio, 50oC warm water extracts, and extraction time 2 times, each 3 h of extraction time, is filtered after extraction, collects plantain seed；Car
Preceding son continues on for follow-up water-bath extraction, Extracting temperature 100oThe quality volume of C, plantain seed and water（kg/L）Than for 1:10,
Extraction time 2 times, each 3 h of extraction time；Extracting solution is centrifuged, and centrifugal rotational speed is controlled in 4800 r/min, centrifugation time
10 min, collect supernatant polysaccharide solution and are concentrated；The ethanol that mass fraction is 95% is added into concentrate to be precipitated,
The final concentration of mass fraction 80% of final ethanol in system, stands 12 more than h and precipitation is collected by centrifugation again, precipitation plus water are answered
It is molten, albumen is taken off using Sevag methods repeatedly, polysaccharide solution is collected and dialyses；Dialyzate is concentrated in vacuo after dialysis, is cold
It is lyophilized dry, obtain plantago asiatica linne polyoses PLCP-3.
10 g plantago asiatica linne polyoses PLCP-3 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For 1:5 ratio
Example dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.05%, is then freeze-dried, gained plantago asiatica linne polyoses
Viscosity significantly reduces.
Embodiment 11.
Weigh a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, 24 h of immersion with
On, plantain seed is collected by filtration, is placed in baking oven dry.Then the above-mentioned plantain seeds of 100 g are weighed and carry out water-bath extraction, extraction
Temperature is 100oC, the mass volume ratio of feed liquid（kg/L）For 1:10, extract 2 times, each extraction time is 3 h, with rotating speed 4800
R/min, 10 min of time centrifuge extracting solution and plantain seed；Merge the supernatant extracted twice, add after vacuum concentration
Enter the ethanol precipitation that mass fraction is 95%, final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；Rotating speed 4800
Precipitation is collected by centrifugation in r/min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gained
Component obtains water-soluble plantago asiatica linne polyoses PLCP-1 after freeze-drying again.Plantain seed after above-mentioned steps are extracted is residual
Slag is dried, then the mass volume ratio of alkali-soluble polysaccharide component, plantain seed and NaOH solution is extracted with NaOH solution（kg/L）For 1:
10,4 DEG C of Extracting temperature, 2 h of extraction time, is extracted 2 times, each extraction time is 3 h, with 4800 r/min of rotating speed, time 10
Min centrifuges extracting solution and plantain seed, adds acetic acid neutralization；Merge the supernatant for extracting, being obtained after neutralization twice, vacuum
Mass fraction is added after concentration as 95% ethanol precipitation, final ethanol mass fraction is 80% in system, is refrigerated at 4 DEG C
Night；Precipitation is collected by centrifugation in 4800 r/min of rotating speed, 10 min of time, is redissolved again in water after freeze-drying, anti-using Sevag methods
Albumen is taken off again, is collected polysaccharide solution and is dialysed；Dialyzate is concentrated in vacuo after dialysis, then toward adding quality in concentrate
Fraction is 95% ethanol precipitation, and final ethanol mass fraction is 80% in system, refrigerated overnight at 4 DEG C；4800 r/ of rotating speed
Precipitation is collected by centrifugation in min, 10 min of time；Precipitation is respectively washed twice with acetone, anhydrous ether and absolute ethyl alcohol successively, gains
Matter obtains alkali solubility plantago asiatica linne polyoses PLCP-2 by freeze-drying again.
10 g plantago asiatica linne polyoses PLCP-1, PLCP-2 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For
1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.2%, is then freeze-dried, gained Chinese herbaceous peony
Sub- polysaccharide viscosity significantly reduces.
Embodiment 12.
Plantain seed is placed in the ethanol that mass fraction is 80% and soaks 12 more than h, for several times, then filtering is received for during which stirring
Collect plantain seed, be placed in drying box dry；Plantain seed is after removal of impurities, by plantain seed and the mass volume ratio of water（kg/L）For 1:10
Ratio, 50oC warm water extracts, and extraction time 2 times, each 3 h of extraction time, is filtered after extraction, collects plantain seed；Car
Preceding son continues on for follow-up water-bath extraction, Extracting temperature 100oThe quality volume of C, plantain seed and water（kg/L）Than for 1:10,
Extraction time 2 times, each 3 h of extraction time；Extracting solution is centrifuged, and centrifugal rotational speed is controlled in 4800 r/min, centrifugation time
10 min, collect supernatant polysaccharide solution and are concentrated；The ethanol that mass fraction is 95% is added into concentrate to be precipitated,
The final concentration of mass fraction 80% of final ethanol in system, stands 12 more than h and precipitation is collected by centrifugation again, precipitation plus water are answered
It is molten, albumen is taken off using Sevag methods repeatedly, polysaccharide solution is collected and dialyses；Dialyzate is concentrated in vacuo after dialysis, is cold
It is lyophilized dry, obtain plantago asiatica linne polyoses PLCP-3.
10 g plantago asiatica linne polyoses PLCP-3 are weighed respectively, according to raw material and aqueous solution mass volume ratio（g/L）For 1:5 ratio
Example dissolving polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.2%, is then freeze-dried, gained plantago asiatica linne polyoses
Viscosity significantly reduces.
With reference in above-mentioned specific embodiment gained sample, to it is of the present invention reduction plantago asiatica linne polyoses stickiness make into
One step explanation.
1st, key instrument and equipment.
ARES G-2 rheometers（TA companies of the U.S.）, Milli-Q ultra-pure water instrument（Millipore companies of the U.S.）Deng.
2nd, test method.
According to described in above-described embodiment, configuration quality fraction is 0.5% various plantago asiatica linne polyoses, is separately added into certain matter
The tea polyphenols of amount, make its mass fraction respectively reach 0.025,0.05% or 0.2%, are then measured using ARES rheometer apparent
Viscosity, shear rate：0.1-1000 s-1, test temperature 25oC。
Or according to described in above-described embodiment, configuration quality fraction is 0.5% various plantago asiatica linne polyoses, is separately added into one
Determine the tea polyphenols of quality, its mass fraction is respectively reached 0.025,0.05% or 0.2%, be then freeze-dried.Gained
Polysaccharide sample adds water to redissolve respectively again, and the volume mass fraction for making polysaccharide is 0.5%, recycles ARES rheometer measure is apparent to stick
Degree, shear rate：0.1-1000 s-1, test temperature 25oC。
3rd, experimental result.
Fig. 1-3 is addition certain mass tea polyphenols in the various plantago asiatica linne polyoses that mass fraction is 0.5%, makes tea polyphenols matter
Amount fraction reaches 0.025,0.05% or 0.2%, then measures apparent viscosity.From measurement result, after adding tea polyphenols, respectively
The plantago asiatica linne polyoses apparent viscosity that kind distinct methods are prepared all significantly reduces.
Fig. 4-6 is the tea polyphenols that certain mass is added in the various plantago asiatica linne polyoses that mass fraction is 0.5%, makes tea polyphenols
Mass fraction reaches 0.025,0.05% or 0.2%, is then freeze-dried, and gained sample measures apparent stick after adding water redissolution
Degree.From measurement result, the various plantago asiatica linne polyoses after tea polyphenols are added, redissolution, apparent viscosity are added water after freeze-drying
Still significantly reduce.
Claims (2)
- A kind of 1. method that plantago asiatica linne polyoses viscosity is reduced using tea polyphenols, it is characterized in that according to the following steps：（1）A certain amount of dry plantain seed is weighed, water-soluble plantago asiatica linne polyoses are prepared using hot water extraction, ethanol precipitation, it is remaining Plantain seed residue is extracted with NaOH again, and extracting solution is concentrated, alcohol precipitation, Sevag methods take off albumen, obtains alkali solubility plantago asiatica linne polyoses；（2）A certain amount of above-mentioned water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses are weighed respectively, according to plantago asiatica linne polyoses With the mass volume ratio of water（g/L）For 1:5 ratio dissolving polysaccharide, adds tea polyphenols, the mass fractions of tea polyphenols for 0.025 ~ 0.2%, water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses are uniformly mixed with tea polyphenols respectively, it is molten to obtain plantago asiatica linne polyoses Liquid.
- A kind of 2. method that plantago asiatica linne polyoses viscosity is reduced using tea polyphenols, it is characterized in that according to the following steps：（1）A certain amount of dry plantain seed is weighed, after extracting low stickiness component with warm water, residue uses boiling waterbath, Ran Houjing again Cross concentration, alcohol precipitation, de- albumen acquisition plantago asiatica linne polyoses；（2）A certain amount of above-mentioned plantago asiatica linne polyoses are weighed, according to plantago asiatica linne polyoses and the mass volume ratio of water（g/L）For 1:5 Ratio dissolves polysaccharide, adds tea polyphenols, the mass fraction of tea polyphenols is 0.025 ~ 0.2%, and above-mentioned polysaccharide is mixed with tea polyphenols It is even, obtain plantago asiatica linne polyoses solution.
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