CN105601948A - Method for reducing viscosity of plantain seed polysaccharide by using tea polyphenol - Google Patents

Method for reducing viscosity of plantain seed polysaccharide by using tea polyphenol Download PDF

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CN105601948A
CN105601948A CN201510887450.1A CN201510887450A CN105601948A CN 105601948 A CN105601948 A CN 105601948A CN 201510887450 A CN201510887450 A CN 201510887450A CN 105601948 A CN105601948 A CN 105601948A
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plantain seed
plantago asiatica
asiatica linne
linne polyoses
tea polyphenols
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CN105601948B (en
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谢明勇
殷军艺
王力
刘晓莹
聂少平
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Nanchang University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/05—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/15—Heterocyclic compounds having oxygen in the ring
    • C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
    • C08K5/1545—Six-membered rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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  • Dispersion Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention provides a method for reducing the viscosity of plantain seed polysaccharide by using tea polyphenol. The method comprises the following steps: (1) weighing a certain amount of dried plantain seeds, preparing water-soluble plantain seed polysaccharide by using hot water extraction and ethanol precipitation methods, then extracting residual plantain seed residues with NaOH and subjecting obtained extract to concentration, alcohol precipitation and Sevag-process protein removal so as to obtain alkali-soluble plantain seed polysaccharide; or extracting low-viscosity components with warm water, then subjecting the residues to extraction in a boiling water bath and carrying out concentration, alcohol precipitation and protein removal so as to obtain plantain seed polysaccharide; and (2) separately weighing the plantain seed polysaccharide obtained in the previous step, dissolving the polysaccharide according to a mass volume ratio of the plantain seed polysaccharide to an aqueous solution of 1: 5, adding tea polyphenol with a mass percentage of 0.025 to 0.2% and uniformly mixing the plantain seed polysaccharide with the tea polyphenol so as to obtain a low-viscosity. According to the invention, after addition of a small amount of the tea polyphenol, the viscosity of the plantain seed polysaccharide solution can be reduced; and the method is applicable to plantain seed polysaccharide prepared by a variety of extraction methods.

Description

A kind of method of utilizing Tea Polyphenols to reduce plantago asiatica linne polyoses viscosity
Technical field
The invention belongs to natural products preparation field.
Background technology
Before plantain seed is Plantaginaceae plant carPlantagoasiaticaL. or before flatcarPlantagoderpressaWilld. dry mature seed, the fruit ear of gathering when seed maturity in summer, two season of autumn, rubs seed, removes impurity and obtain, and is classified as by food and medicine Surveillance Authority of China the article that can be used for health food. " plantain seed taste is sweet cold nontoxic; The infirmity pain relieving of main gas, sharp water diuresis, except arthritis with fixed pain caused by dampness; For a long time clothes are made light of one's life by commiting suicide resistance to old ", be China ancient times the earliest and one of the most widely used certified products medicinal material.
From plantain seed, extracting the main polysaccharide obtaining, is a kind of composition that is rich in araboxylan, and viscosity is very high, just can form weak gel when polysaccharide concentration is slightly higher. Modern study shows, plantago asiatica linne polyoses has many functional activities, comprise antioxygen, hypoglycemic, reducing blood lipid and regulate body's immunity etc., plantago asiatica linne polyoses high viscosity feature simultaneously, give it and relax bowel, promote intestinal health, increase the physiological functions such as ight soil water content, and can play special roles such as removing heavy metal of body. But high viscosity feature is also for its production and application have increased inconvenience, particularly the solubility that adds water of polyose after dry is produced to considerable influence, can increase the energy consumption in plantago asiatica linne polyoses production, preparation process, this problem is subject to people's common concern all the time but makes slow progress simultaneously. Therefore, need to, by certain technology and method, effectively reduce plantago asiatica linne polyoses viscosity, ensure low cost simultaneously, the further development and utilization that promotes plantago asiatica linne polyoses with this, increases economic benefit.
Summary of the invention
The object of the present invention is to provide one to utilize Tea Polyphenols to reduce the method for plantago asiatica linne polyoses (PlantagoasiaticaL.CrudePolysaccharide, PLCP) viscosity.
The present invention is achieved by the following technical solutions.
The present invention according to the following steps.
(1) plantago asiatica linne polyoses preparation: take a certain amount of dry plantain seed, adopt hot water lixiviate, ethanol precipitation to prepare water-soluble plantago asiatica linne polyoses, residue plantain seed residue extracts with NaOH again, and extract, through steps such as concentrated, alcohol precipitation, the de-albumen of Sevag method, obtains alkali solubility plantago asiatica linne polyoses.
(2) low viscosity plantago asiatica linne polyoses preparation: take respectively a certain amount of above-mentioned water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses, the ratio that is 1:5 according to plantago asiatica linne polyoses and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, add Tea Polyphenols, the mass fraction of Tea Polyphenols is 0.025 ~ 0.2%, after respectively water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses being mixed with Tea Polyphenols, obtain low-viscosity plantago asiatica linne polyoses solution.
The present invention can also be according to the following steps.
(1) take a certain amount of dry plantain seed, extract after low stickiness component with warm water, residue is used boiling waterbath again, then obtains plantago asiatica linne polyoses through steps such as concentrated, alcohol precipitation, de-albumen.
(2) take a certain amount of above-mentioned plantago asiatica linne polyoses, the ratio that is 1:5 according to plantago asiatica linne polyoses and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, add Tea Polyphenols, the mass fraction of Tea Polyphenols is 0.025 ~ 0.2%, above-mentioned polysaccharide is mixed with Tea Polyphenols, obtain low-viscosity plantago asiatica linne polyoses solution.
Plantago asiatica linne polyoses of the present invention can be also commercially available or other method is extracted the plantago asiatica linne polyoses of preparation.
Advantage of the present invention is: after 1, adding a small amount of Tea Polyphenols, just can significantly reduce plantago asiatica linne polyoses solution viscosity; 2, be applicable to the plantago asiatica linne polyoses that various extracting methods prepare; 3, add a small amount of Tea Polyphenols to mix with plantago asiatica linne polyoses solution after super-dry again, still can effectively reduce polysaccharide solution viscosity, the effect of redissolving that adds water is better than undressed polysaccharide former state.
Brief description of the drawings
Fig. 1 is the impacts of different Tea Polyphenols additions on plantago asiatica linne polyoses PLCP-1 apparent viscosity.
Fig. 2 is the impacts of different Tea Polyphenols additions on plantago asiatica linne polyoses PLCP-2 apparent viscosity.
Fig. 3 is the impacts of different Tea Polyphenols additions on plantago asiatica linne polyoses PLCP-3 apparent viscosity.
Fig. 4 is the impact of different Tea Polyphenols additions on plantago asiatica linne polyoses PLCP-1 apparent viscosity (polysaccharide adds first freeze drying after Tea Polyphenols, and then add water redissolve test).
Fig. 5 is the impact of different Tea Polyphenols additions on plantago asiatica linne polyoses PLCP-2 apparent viscosity (polysaccharide adds first freeze drying after Tea Polyphenols, and then add water redissolve test).
Fig. 6 is the impact of different Tea Polyphenols additions on plantago asiatica linne polyoses PLCP-3 apparent viscosity (polysaccharide adds first freeze drying after Tea Polyphenols, and then add water redissolve test).
Detailed description of the invention
Below by embodiment, technical scheme of the present invention is clearly and completely described, described embodiment is only the present invention's part embodiment, instead of whole embodiment. Based on the embodiment in the present invention, those skilled in the art, not making other embodiment that obtain under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1.
Take a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, more than soaking 24h, filters and collects plantain seed, is placed in baking oven dry. Then take the above-mentioned plantain seed of 100g and carry out water-bath extraction, extracting temperature is 100oC, the mass volume ratio (kg/L) of feed liquid is 1:10, extracts 2 times, each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed; Merge the supernatant that obtains of extracted twice, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and obtained component obtains water-soluble plantago asiatica linne polyoses PLCP-1 again after freeze drying. Plantain seed residue after above-mentioned steps is extracted is dry, extract alkali-soluble polysaccharide component with NaOH solution again, the mass volume ratio (kg/L) of plantain seed and NaOH solution is 1:10, extract 4 DEG C of temperature, extraction time 2h, extracts 2 times, and each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed, then add acetic acid neutralization; Merge the supernatant that obtains after extracted twice, neutralization, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation, multiple water-soluble again after freeze drying, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After dialysis finishes, by dislysate Vacuum Concentration, then be 95% ethanol precipitation toward adding mass fraction in concentrate, in system, final ethanol mass fraction is to refrigerate and spend the night at 80%, 4 DEG C; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and gained material obtains alkali solubility plantago asiatica linne polyoses PLCP-2 through freeze drying again.
Take respectively 10g plantago asiatica linne polyoses PLCP-1, PLCP-2, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.025%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 2.
It is more than 80% ethanol soaks 12h that plantain seed is placed in to mass fraction, stirs during this time for several times, then filters and collects plantain seed, is placed in drying box dry; Plantain seed after removal of impurities, the ratio that is 1:10 in the mass volume ratio of plantain seed and water (kg/L), 50oC warm water extracts, extraction time 2 times, and each extraction time 3h, extracts and finishes rear filtration, collects plantain seed; Plantain seed continues on for follow-up water-bath and extracts, and extracting temperature is 100oC, quality volume (kg/L) ratio of plantain seed and water is 1:10, extraction time 2 times, each extraction time 3h; Extract carries out centrifugal, and centrifugal rotational speed is controlled at 4800r/min, and centrifugation time 10min collects supernatant polysaccharide solution and concentrates; Be that 95% ethanol precipitates toward adding mass fraction in concentrate, in system, the final concentration of final ethanol is mass fraction 80%, standing 12h centrifugal collecting precipitation more above, the precipitation redissolution that adds water, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After finishing, dialysis by dislysate Vacuum Concentration, freeze drying, obtains plantago asiatica linne polyoses PLCP-3.
Take 10g plantago asiatica linne polyoses PLCP-3, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.025%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 3.
Take a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, more than soaking 24h, filters and collects plantain seed, is placed in baking oven dry. Then take the above-mentioned plantain seed of 100g and carry out water-bath extraction, extracting temperature is 100oC, the mass volume ratio (kg/L) of feed liquid is 1:10, extracts 2 times, each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed; Merge the supernatant that obtains of extracted twice, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and obtained component obtains water-soluble plantago asiatica linne polyoses PLCP-1 again after freeze drying. Plantain seed residue after above-mentioned steps is extracted is dry, extract alkali-soluble polysaccharide component with NaOH solution again, the mass volume ratio (kg/L) of plantain seed and NaOH solution is 1:10, extract 4 DEG C of temperature, extraction time 2h, extracts 2 times, and each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed, then add acetic acid neutralization; Merge the supernatant that obtains after extracted twice, neutralization, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation, multiple water-soluble again after freeze drying, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After dialysis finishes, by dislysate Vacuum Concentration, then be 95% ethanol precipitation toward adding mass fraction in concentrate, in system, final ethanol mass fraction is to refrigerate and spend the night at 80%, 4 DEG C; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and gained material obtains alkali solubility plantago asiatica linne polyoses PLCP-2 through freeze drying again.
Take respectively 10g plantago asiatica linne polyoses PLCP-1, PLCP-2, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.05%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 4.
It is more than 80% ethanol soaks 12h that plantain seed is placed in to mass fraction, stirs during this time for several times, then filters and collects plantain seed, is placed in drying box dry; Plantain seed after removal of impurities, the ratio that is 1:10 in the mass volume ratio of plantain seed and water (kg/L), 50oC warm water extracts, extraction time 2 times, and each extraction time 3h, extracts and finishes rear filtration, collects plantain seed; Plantain seed continues on for follow-up water-bath and extracts, and extracting temperature is 100oC, quality volume (kg/L) ratio of plantain seed and water is 1:10, extraction time 2 times, each extraction time 3h; Extract carries out centrifugal, and centrifugal rotational speed is controlled at 4800r/min, and centrifugation time 10min collects supernatant polysaccharide solution and concentrates; Be that 95% ethanol precipitates toward adding mass fraction in concentrate, in system, the final concentration of final ethanol is mass fraction 80%, standing 12h centrifugal collecting precipitation more above, the precipitation redissolution that adds water, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After finishing, dialysis by dislysate Vacuum Concentration, freeze drying, obtains plantago asiatica linne polyoses PLCP-3.
Take 10g plantago asiatica linne polyoses PLCP-3, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.05%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 5.
Take a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, more than soaking 24h, filters and collects plantain seed, is placed in baking oven dry. Then take the above-mentioned plantain seed of 100g and carry out water-bath extraction, extracting temperature is 100oC, the mass volume ratio (kg/L) of feed liquid is 1:10, extracts 2 times, each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed; Merge the supernatant that obtains of extracted twice, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and obtained component obtains water-soluble plantago asiatica linne polyoses PLCP-1 again after freeze drying. Plantain seed residue after above-mentioned steps is extracted is dry, extract alkali-soluble polysaccharide component with NaOH solution again, the mass volume ratio (kg/L) of plantain seed and NaOH solution is 1:10, extract 4 DEG C of temperature, extraction time 2h, extracts 2 times, and each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed, then add acetic acid neutralization; Merge the supernatant that obtains after extracted twice, neutralization, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation, multiple water-soluble again after freeze drying, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After dialysis finishes, by dislysate Vacuum Concentration, then be 95% ethanol precipitation toward adding mass fraction in concentrate, in system, final ethanol mass fraction is to refrigerate and spend the night at 80%, 4 DEG C; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and gained material obtains alkali solubility plantago asiatica linne polyoses PLCP-2 through freeze drying again.
Take respectively 10g plantago asiatica linne polyoses PLCP-1, PLCP-2, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.2%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 6.
It is more than 80% ethanol soaks 12h that plantain seed is placed in to mass fraction, stirs during this time for several times, then filters and collects plantain seed, is placed in drying box dry; Plantain seed after removal of impurities, the ratio that is 1:10 in the mass volume ratio of plantain seed and water (kg/L), 50oC warm water extracts, extraction time 2 times, and each extraction time 3h, extracts and finishes rear filtration, collects plantain seed; Plantain seed continues on for follow-up water-bath and extracts, and extracting temperature is 100oC, quality volume (kg/L) ratio of plantain seed and water is 1:10, extraction time 2 times, each extraction time 3h; Extract carries out centrifugal, and centrifugal rotational speed is controlled at 4800r/min, and centrifugation time 10min collects supernatant polysaccharide solution and concentrates; Be that 95% ethanol precipitates toward adding mass fraction in concentrate, in system, the final concentration of final ethanol is mass fraction 80%, standing 12h centrifugal collecting precipitation more above, the precipitation redissolution that adds water, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After finishing, dialysis by dislysate Vacuum Concentration, freeze drying, obtains plantago asiatica linne polyoses PLCP-3.
Take 10g plantago asiatica linne polyoses PLCP-3, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.2%, can significantly reduce plantago asiatica linne polyoses viscosity.
Embodiment 7.
Take a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, more than soaking 24h, filters and collects plantain seed, is placed in baking oven dry. Then take the above-mentioned plantain seed of 100g and carry out water-bath extraction, extracting temperature is 100oC, the mass volume ratio (kg/L) of feed liquid is 1:10, extracts 2 times, each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed; Merge the supernatant that obtains of extracted twice, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and obtained component obtains water-soluble plantago asiatica linne polyoses PLCP-1 again after freeze drying. Plantain seed residue after above-mentioned steps is extracted is dry, extract alkali-soluble polysaccharide component with NaOH solution again, the mass volume ratio (kg/L) of plantain seed and NaOH solution is 1:10, extract 4 DEG C of temperature, extraction time 2h, extracts 2 times, and each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed, then add acetic acid neutralization; Merge the supernatant that obtains after extracted twice, neutralization, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation, multiple water-soluble again after freeze drying, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After dialysis finishes, by dislysate Vacuum Concentration, then be 95% ethanol precipitation toward adding mass fraction in concentrate, in system, final ethanol mass fraction is to refrigerate and spend the night at 80%, 4 DEG C; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and gained material obtains alkali solubility plantago asiatica linne polyoses PLCP-2 through freeze drying again.
Take respectively 10g plantago asiatica linne polyoses PLCP-1, PLCP-2, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.025%, then carry out freeze drying, gained plantago asiatica linne polyoses viscosity significantly reduces.
Embodiment 8.
It is more than 80% ethanol soaks 12h that plantain seed is placed in to mass fraction, stirs during this time for several times, then filters and collects plantain seed, is placed in drying box dry; Plantain seed after removal of impurities, the ratio that is 1:10 in the mass volume ratio of plantain seed and water (kg/L), 50oC warm water extracts, extraction time 2 times, and each extraction time 3h, extracts and finishes rear filtration, collects plantain seed; Plantain seed continues on for follow-up water-bath and extracts, and extracting temperature is 100oC, quality volume (kg/L) ratio of plantain seed and water is 1:10, extraction time 2 times, each extraction time 3h; Extract carries out centrifugal, and centrifugal rotational speed is controlled at 4800r/min, and centrifugation time 10min collects supernatant polysaccharide solution and concentrates; Be that 95% ethanol precipitates toward adding mass fraction in concentrate, in system, the final concentration of final ethanol is mass fraction 80%, standing 12h centrifugal collecting precipitation more above, the precipitation redissolution that adds water, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After finishing, dialysis by dislysate Vacuum Concentration, freeze drying, obtains plantago asiatica linne polyoses PLCP-3.
Take respectively 10g plantago asiatica linne polyoses PLCP-3, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.025%, then carry out freeze drying, gained plantago asiatica linne polyoses viscosity significantly reduces.
Embodiment 9.
Take a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, more than soaking 24h, filters and collects plantain seed, is placed in baking oven dry. Then take the above-mentioned plantain seed of 100g and carry out water-bath extraction, extracting temperature is 100oC, the mass volume ratio (kg/L) of feed liquid is 1:10, extracts 2 times, each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed; Merge the supernatant that obtains of extracted twice, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and obtained component obtains water-soluble plantago asiatica linne polyoses PLCP-1 again after freeze drying. Plantain seed residue after above-mentioned steps is extracted is dry, extract alkali-soluble polysaccharide component with NaOH solution again, the mass volume ratio (kg/L) of plantain seed and NaOH solution is 1:10, extract 4 DEG C of temperature, extraction time 2h, extracts 2 times, and each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed, then add acetic acid neutralization; Merge the supernatant that obtains after extracted twice, neutralization, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation, multiple water-soluble again after freeze drying, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After dialysis finishes, by dislysate Vacuum Concentration, then be 95% ethanol precipitation toward adding mass fraction in concentrate, in system, final ethanol mass fraction is to refrigerate and spend the night at 80%, 4 DEG C; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and gained material obtains alkali solubility plantago asiatica linne polyoses PLCP-2 through freeze drying again.
Take respectively 10g plantago asiatica linne polyoses PLCP-1, PLCP-2, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.05%, then carry out freeze drying, gained plantago asiatica linne polyoses viscosity significantly reduces.
Embodiment 10.
It is more than 80% ethanol soaks 12h that plantain seed is placed in to mass fraction, stirs during this time for several times, then filters and collects plantain seed, is placed in drying box dry; Plantain seed after removal of impurities, the ratio that is 1:10 in the mass volume ratio of plantain seed and water (kg/L), 50oC warm water extracts, extraction time 2 times, and each extraction time 3h, extracts and finishes rear filtration, collects plantain seed; Plantain seed continues on for follow-up water-bath and extracts, and extracting temperature is 100oC, quality volume (kg/L) ratio of plantain seed and water is 1:10, extraction time 2 times, each extraction time 3h; Extract carries out centrifugal, and centrifugal rotational speed is controlled at 4800r/min, and centrifugation time 10min collects supernatant polysaccharide solution and concentrates; Be that 95% ethanol precipitates toward adding mass fraction in concentrate, in system, the final concentration of final ethanol is mass fraction 80%, standing 12h centrifugal collecting precipitation more above, the precipitation redissolution that adds water, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After finishing, dialysis by dislysate Vacuum Concentration, freeze drying, obtains plantago asiatica linne polyoses PLCP-3.
Take respectively 10g plantago asiatica linne polyoses PLCP-3, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.05%, then carry out freeze drying, gained plantago asiatica linne polyoses viscosity significantly reduces.
Embodiment 11.
Take a certain amount of dry plantain seed, add the ethanol of 10 times of volumes, ethanol mass fraction is 80%, more than soaking 24h, filters and collects plantain seed, is placed in baking oven dry. Then take the above-mentioned plantain seed of 100g and carry out water-bath extraction, extracting temperature is 100oC, the mass volume ratio (kg/L) of feed liquid is 1:10, extracts 2 times, each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed; Merge the supernatant that obtains of extracted twice, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and obtained component obtains water-soluble plantago asiatica linne polyoses PLCP-1 again after freeze drying. Plantain seed residue after above-mentioned steps is extracted is dry, extract alkali-soluble polysaccharide component with NaOH solution again, the mass volume ratio (kg/L) of plantain seed and NaOH solution is 1:10, extract 4 DEG C of temperature, extraction time 2h, extracts 2 times, and each extraction time is 3h, with rotating speed 4800r/min, time 10min centrifugation extract and plantain seed, then add acetic acid neutralization; Merge the supernatant that obtains after extracted twice, neutralization, after Vacuum Concentration, adding mass fraction is 95% ethanol precipitation, and in system, final ethanol mass fraction is that at 80%, 4 DEG C, refrigeration is spent the night; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation, multiple water-soluble again after freeze drying, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After dialysis finishes, by dislysate Vacuum Concentration, then be 95% ethanol precipitation toward adding mass fraction in concentrate, in system, final ethanol mass fraction is to refrigerate and spend the night at 80%, 4 DEG C; Rotating speed 4800r/min, time 10min centrifugal collecting precipitation; Precipitation is used the each washed twice of acetone, absolute ether and absolute ethyl alcohol successively, and gained material obtains alkali solubility plantago asiatica linne polyoses PLCP-2 through freeze drying again.
Take respectively 10g plantago asiatica linne polyoses PLCP-1, PLCP-2, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.2%, then carry out freeze drying, gained plantago asiatica linne polyoses viscosity significantly reduces.
Embodiment 12.
It is more than 80% ethanol soaks 12h that plantain seed is placed in to mass fraction, stirs during this time for several times, then filters and collects plantain seed, is placed in drying box dry; Plantain seed after removal of impurities, the ratio that is 1:10 in the mass volume ratio of plantain seed and water (kg/L), 50oC warm water extracts, extraction time 2 times, and each extraction time 3h, extracts and finishes rear filtration, collects plantain seed; Plantain seed continues on for follow-up water-bath and extracts, and extracting temperature is 100oC, quality volume (kg/L) ratio of plantain seed and water is 1:10, extraction time 2 times, each extraction time 3h; Extract carries out centrifugal, and centrifugal rotational speed is controlled at 4800r/min, and centrifugation time 10min collects supernatant polysaccharide solution and concentrates; Be that 95% ethanol precipitates toward adding mass fraction in concentrate, in system, the final concentration of final ethanol is mass fraction 80%, standing 12h centrifugal collecting precipitation more above, the precipitation redissolution that adds water, adopt Sevag method de-albumen repeatedly, collect polysaccharide solution and dialyse; After finishing, dialysis by dislysate Vacuum Concentration, freeze drying, obtains plantago asiatica linne polyoses PLCP-3.
Take respectively 10g plantago asiatica linne polyoses PLCP-3, the ratio that is 1:5 according to raw material and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, adds Tea Polyphenols, and the mass fraction of Tea Polyphenols is 0.2%, then carry out freeze drying, gained plantago asiatica linne polyoses viscosity significantly reduces.
Below in conjunction with gained sample in above-mentioned specific embodiment, reduction plantago asiatica linne polyoses stickiness of the present invention is described further.
1, key instrument and equipment.
ARESG-2 flow graph (TA company of the U.S.), Milli-Q ultra-pure water instrument (Millipore company of the U.S.) etc.
2, method of testing.
Described in above-described embodiment, configuration quality mark is 0.5% various plantago asiatica linne polyoses, adds respectively the Tea Polyphenols of certain mass, makes its mass fraction reach respectively 0.025,0.05% or 0.2%, then utilize ARES rheometer measurement apparent viscosity, shear rate: 0.1-1000s-1, probe temperature is 25oC。
Or described in above-described embodiment, the various plantago asiatica linne polyoses that configuration quality mark is 0.5%, add respectively the Tea Polyphenols of certain mass, make its mass fraction reach respectively 0.025,0.05% or 0.2%, then carry out freeze drying. The redissolution that adds water respectively again of gained polysaccharide sample, the volume mass mark that makes polysaccharide is 0.5%, recycling ARES rheometer measurement apparent viscosity, shear rate: 0.1-1000s-1, probe temperature is 25oC。
3, experimental result.
Fig. 1-3, for adding certain mass Tea Polyphenols in the mass fraction various plantago asiatica linne polyoses that are 0.5%, make Tea Polyphenols mass fraction reach 0.025,0.05% or 0.2%, then measure apparent viscosity. From measurement result, add after Tea Polyphenols, the plantago asiatica linne polyoses apparent viscosity that various distinct methods prepare all significantly reduces.
Fig. 4-6, for adding the Tea Polyphenols of certain mass in the mass fraction various plantago asiatica linne polyoses that are 0.5%, make Tea Polyphenols mass fraction reach 0.025,0.05% or 0.2%, then freeze drying, and gained sample is measured apparent viscosity after adding water and redissolving. From measurement result, add the various plantago asiatica linne polyoses after Tea Polyphenols, the redissolution that adds water again after freeze drying, apparent viscosity still significantly reduces.

Claims (2)

1. utilize Tea Polyphenols to reduce a method for plantago asiatica linne polyoses viscosity, it is characterized in that according to the following steps:
(1) take a certain amount of dry plantain seed, adopt hot water lixiviate, ethanol precipitation to prepare water-soluble plantago asiatica linne polyoses, residue plantain seed residue extracts with NaOH again, and extract, through concentrated, alcohol precipitation, the de-albumen of Sevag method, obtains alkali solubility plantago asiatica linne polyoses;
(2) take respectively a certain amount of above-mentioned water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses, the ratio that is 1:5 according to plantago asiatica linne polyoses and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, add Tea Polyphenols, the mass fraction of Tea Polyphenols is 0.025 ~ 0.2%, respectively water-soluble plantago asiatica linne polyoses or alkali solubility plantago asiatica linne polyoses are mixed with Tea Polyphenols, obtain low-viscosity plantago asiatica linne polyoses solution.
2. utilize Tea Polyphenols to reduce a method for plantago asiatica linne polyoses viscosity, it is characterized in that according to the following steps:
(1) take a certain amount of dry plantain seed, extract after low stickiness component with warm water, residue is used boiling waterbath again, then obtains plantago asiatica linne polyoses through concentrated, alcohol precipitation, de-albumen;
(2) take a certain amount of above-mentioned plantago asiatica linne polyoses, the ratio that is 1:5 according to plantago asiatica linne polyoses and aqueous solution mass volume ratio (g/L) is dissolved polysaccharide, add Tea Polyphenols, the mass fraction of Tea Polyphenols is 0.025 ~ 0.2%, above-mentioned polysaccharide is mixed with Tea Polyphenols, obtain low-viscosity plantago asiatica linne polyoses solution.
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CN116649563A (en) * 2023-06-19 2023-08-29 浙江大学长三角智慧绿洲创新中心 Food additive for dispersing ganoderma lucidum powder and rapid ganoderma lucidum powder dispersing method

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CN105028603A (en) * 2015-05-18 2015-11-11 浙江海洋学院 Oligosaccharide water-retaining agent used for water retention of red shrimps and use method thereof
CN105037571A (en) * 2015-06-30 2015-11-11 南昌大学 Method for preparing low-viscosity Semen plantaginis polysaccharides through enzyme technology

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CN105028603A (en) * 2015-05-18 2015-11-11 浙江海洋学院 Oligosaccharide water-retaining agent used for water retention of red shrimps and use method thereof
CN105037571A (en) * 2015-06-30 2015-11-11 南昌大学 Method for preparing low-viscosity Semen plantaginis polysaccharides through enzyme technology

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CN113974158A (en) * 2021-10-15 2022-01-28 江西仙客来生物科技有限公司 Ganoderma lucidum, agaricus blazei murill and epimedium oral liquid
CN116649563A (en) * 2023-06-19 2023-08-29 浙江大学长三角智慧绿洲创新中心 Food additive for dispersing ganoderma lucidum powder and rapid ganoderma lucidum powder dispersing method
CN116649563B (en) * 2023-06-19 2024-05-28 浙江大学长三角智慧绿洲创新中心 Food additive for dispersing ganoderma lucidum powder and rapid ganoderma lucidum powder dispersing method

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