CN106220748A - A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method - Google Patents
A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method Download PDFInfo
- Publication number
- CN106220748A CN106220748A CN201610624969.5A CN201610624969A CN106220748A CN 106220748 A CN106220748 A CN 106220748A CN 201610624969 A CN201610624969 A CN 201610624969A CN 106220748 A CN106220748 A CN 106220748A
- Authority
- CN
- China
- Prior art keywords
- salicornia bigelovii
- bigelovii torr
- supernatant
- total flavones
- polysaccharide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Sustainable Development (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Biotechnology (AREA)
- Alternative & Traditional Medicine (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medical Informatics (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to the extraction of active components of plants, particularly relate to a kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method, comprise the following steps: S1. Salicornia Bigelovii Torr., clean, be dried, pulverize, sieve, obtain Salicornia Bigelovii Torr. dry powder;S2. weigh dry powder and add distilled water, adjusting pH value, adding enzymolysis under the conditions of compound enzyme vacuum tightness, extraction, be centrifuged, be filtrated to get supernatant a and filtering residue;S3. taking supernatant a to concentrate, extract extracts, and separates to obtain supernatant b;S4. supernatant b is concentrated, add ethanol, extract, be centrifuged, be filtrated to get supernatant c and deposit, through concentrating, being dried to obtain total flavones crude product;S5. adsorbed by macroporous resin column, ethanol elution, collect eluent, concentrate, be dried to obtain Refined flavonoid powder;S6. deposit by enzyme process removing protein, dialyse, be dried to obtain refined polysaccharide.Present invention process is simple, and easy to operate, the time is short, and effectively removes chlorophyll, salinity and other miscellaneous point, improves total flavones and the yield of polysaccharide and product purity.
Description
Technical field
The present invention relates to the extraction of active components of plants, particularly relate to a kind of Salicornia Bigelovii Torr. total flavones and the polysaccharide comprehensively side of extraction
Method.
Background technology
Salicornia Bigelovii Torr. (Salicornia) be Chenopodiaceae salicornia europaeal belong to without the Carnified euhalophyte of base of leaf, tolerance of salinity height,
It is commonly called as marine borer grass, salicornia europaeal, sea covering or sea bean, is more common in lick, seabeach is taken up in salt lake.Recently as both at home and abroad to sea
Deepening continuously of Germinatus Phragmitis research, from Salicornia Bigelovii Torr., isolated polysaccharide, chromocor compound, biogenic salt, chlorophyll etc. are multiple
There is the active component of medical value and health value.Show that chromocor compound has vessel softening, blood sugar lowering, fall by research
Blood fat, antioxidation, removing interior free yl, defying age, resisting pathogenic microbes, infection, anti-inflammatory, antiulcer, antiallergic, rush
Enter the different physiological roles such as tissue regeneration;Polysaccharide has antitumor, antiviral, antiulcer, radioprotective, enhancing immunity, resisting fatigue
Etc. effect.
Chromocor compound, general employing organic solvent method or microwave-assisted organic solvent extraction is extracted at present from Salicornia Bigelovii Torr.
Method, through decolouring, isolated and purified, be dried to obtain flavone product.But use said method to extract chromocor compound to exist
Problem: extraction time length, Extraction solvent consumption are big, and the cell wall that chromocor compound is master with cellulose is surrounded, and
Iuntercellular has pectin to bond, and can hinder solute mass transfer during extraction, causes chromocor compound extraction ratio low, and chromocor compound produces
Product purity is low.Although prior art also has employing to use enzymatic isolation method to extract flavonoid substance from other raw materials, but uses enzymolysis
When method extracts flavone, enzymolysis time is long, reaction time consumption, and extraction ratio is low.
The extracting method of polysaccharide has multiple, extracts polysaccharide material at present from Salicornia Bigelovii Torr., and general employing ultrasonic assistant carries
Follow the example of, through alcohol analysis, deproteinization, dialyse, the link such as be dried and obtain polyose.Although utilizing ultra sonic machinery vibration to produce
Energy, makes medium structure change to a certain extent, promotes effective ingredient to rapidly enter in solvent, but plant cell wall
Structure comparison is firm, and the extraction ratio of polysaccharide material is low, in addition at present polysaccharide deproteinization time, general use Sevage method, TCA method and
NaOH method all can cause the loss of polysaccharide component.Therefore the present invention extracts problem existing for flavone and polysaccharide based on prior art,
Set up a kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method.
Summary of the invention
The technical problem to be solved is: the deficiency existed for prior art, it is provided that a kind of Salicornia Bigelovii Torr. flavone
And polysaccharide combined extraction method, this method technique is simple, and easy to operate, the time is short, can improve again chromocor compound, polysaccharide material simultaneously
The extraction ratio of matter and purity.
For solving above-mentioned technical problem, the technical scheme is that
A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method, described extracting method comprises the following steps:
S1. pluck the fresh leaf of Salicornia Bigelovii Torr., through over cleaning, dry, pulverizing, obtain Salicornia Bigelovii Torr. dry powder;
S2. weigh the Salicornia Bigelovii Torr. dry powder in S1 and add the distilled water of described Salicornia Bigelovii Torr. dry powder weight 10-18 times, adjusting pH value
Between 4.8-6, addition compound enzyme enzymolysis 15-25min under the conditions of the vacuum tightness of 100-200mpa, through homogenate extraction
After, it is centrifuged, is filtrated to get supernatant a and filtering residue;
S3. the supernatant a taking S2 gained concentrates, and then adds the extract of concentrated solution volume 1-3 times, stirs, stands,
It is extracted liquid layer and supernatant layer, is isolated to supernatant b;
S4. the supernatant b obtained by S3 concentrates, and the volumetric concentration then adding concentrated solution volume 6-10 times is 60%-
The ethanol of 80%, extracts 1-3h, is centrifuged, is filtrated to get supernatant c and deposit, then by supernatant c concentration, lyophilization
Obtain total flavones crude product;
S5. the total flavones crude product obtained by S4, dissolves with distilled water, then crosses macroporous resin column, and by volumetric concentration is
The ethanol of 50%-75% carries out eluting to it, collects eluent, then eluent concentration, lyophilization is obtained Refined flavonoid powder;
S6. the deposit distilled water obtained by S4 dissolves, and is subsequently adding the Fructus Chaenomelis of deposit weight 0.1-0.2%
Protease, and adjust pH value of solution for neutrality, hydrolyzes 0.5-1h under the conditions of 60-70 DEG C, enzyme denaturing, dialyse, concentrate, obtain essence after drying
Polysaccharide processed.
As the technical scheme of a kind of improvement, described homogenate extraction condition: extraction time 0.5-2min, Extracting temperature 25-
45 DEG C, extract voltage 110-150V.
As the preferred technical scheme of one, the addition of described compound enzyme is described Salicornia Bigelovii Torr. dry powder weight
0.02%-0.05%.
As the technical scheme of a kind of improvement, described compound enzyme is cellulase, hemicellulase and pectase, and described
The ratio of cellulase, hemicellulase and pectase is 0.6-1.3:0.7-1:0.5-0.7.
As the preferred technical scheme of one, the hydrolysis temperature of described enzymolysis is 40-65 DEG C.
As the technical scheme of a kind of improvement, take the filtering residue that S2 obtains, then with 60% ethanol, homogenate extraction, centrifugal,
Filtering, the filtrate obtained merges with described supernatant a.
As the preferred technical scheme of one, the concentration of the ethanol in described S4 is 70%.
As the preferred technical scheme of one, in described S5, macroporous resin column selects AB-8, HPD-722 or D101-B.
As the preferred technical scheme of one, the extract in described S3 is petroleum ether, chloroform, normal hexane or acetic acid second
Ester.
As a kind of further preferred technical scheme, the extract in described S3 is chloroform.
After have employed technique scheme, the invention has the beneficial effects as follows:
Compared with prior art, the present invention mainly has the advantage that
(1) use compound enzyme, under high pressure vacuum airtight condition, Salicornia Bigelovii Torr. is carried out enzymolysis, enzymolysis time can be shortened, simultaneously
Enzymolysis solution and Extraction solvent quickly enter when boosting in the internal vascular bundle of Salicornia Bigelovii Torr. and glandular cell, make the flavone in cell wall and
Polysaccharide discharges completely, then uses homogenate extraction that effective ingredient can be made to be quickly transferred in Extraction solvent, and extraction time is short,
Improve the extraction ratio of total flavones simultaneously, extracting flavonoids rate can be made to reach 258mg/g;By macroporous resin column to chromocor compound
Being enriched with, flavone crude product is separated by elution further, purification, improves the purity of chromocor compound, and purification
In rear extract, the flavones content of Salicornia Bigelovii Torr. reaches 85.6%;
(2) can effectively remove chlorophyll by extract extraction, remove salt through alcohol steep, protease removing protein, dialysis
Grade small-molecule substance, and available refined polysaccharide, polysaccharide extract rate reaches 52.6mg/g, and purity reaches 86.3%;
(3) present invention takes full advantage of Salicornia Bigelovii Torr. resource, realizes again the extraction to polysaccharide, technique letter while extracting flavone
Single, easy to operate, organic solvent toxicity is little, easy recovery, feasibility are good.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Example 1
A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method thereof, comprise the following steps:
S1. pluck the fresh leaf of Salicornia Bigelovii Torr., through over cleaning, be dried, pulverized 20 mesh sieves, obtain Salicornia Bigelovii Torr. dry powder;
S2. weighing the Salicornia Bigelovii Torr. dry powder in S1 and add the distilled water of described Salicornia Bigelovii Torr. dry powder weight 10 times, tune pH value is
4.8, add 0.02% compound enzyme (ratio of cellulase, hemicellulase and pectase is 0.6:1:0.7) and at 100mpa
Vacuum tightness under the conditions of enzymolysis 25min, and hydrolysis temperature controls at 40 DEG C, and through homogenate extraction, (extraction time 0.5min, carries
Take temperature 30 DEG C, extract voltage 110V), it is centrifuged, is filtrated to get supernatant a and filtering residue;
S3. the supernatant a taking S2 gained concentrates, and then adds the extract (petroleum ether) of concentrated solution volume 1.5 times, stirs
Mix, stand, be extracted liquid layer and supernatant layer, be isolated to supernatant b;
S4. the supernatant b obtained by S3 concentrates, and then adds the second that volumetric concentration is 60% of concentrated solution volume 6 times
Alcohol, extracts 1.5h, is centrifuged, is filtrated to get supernatant b and deposit, then supernatant c concentration, lyophilization is obtained total Huang
Ketone crude product;
S5. the total flavones crude product obtained by S4, dissolves with distilled water, then crosses macroporous resin column (HPD-722), first with steaming
Distilled water eluting, then carries out eluting, eluent flow rate 1ml/min with the ethanol that volumetric concentration is 60% to it, collects ethanol and wash
The eluent flowed out time de-, then obtains refined total flavonoids by eluent concentration, lyophilization;
S6. the deposit distilled water obtained by S4 dissolves, and is subsequently adding the Papain of deposit weight 0.1%
Enzyme, and adjust pH value of solution for neutrality, hydrolyze 0.5h, enzyme denaturing under the conditions of 60 DEG C, dialyse 24h with tap water, use distilled water the most again
Dialysis 12h, concentrates, obtains refined polysaccharide after drying.
Under these process conditions, in Salicornia Bigelovii Torr., total flavones extraction ratio is 239mg/g, and purity is 82.9%;The extraction ratio of polysaccharide
43.5mg/g, purity is 82.4%.
Example 2
A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method thereof, comprise the following steps:
S1. pluck the fresh leaf of Salicornia Bigelovii Torr., through over cleaning, be dried, pulverized 40 mesh sieves, obtain Salicornia Bigelovii Torr. dry powder;
S2. weighing the Salicornia Bigelovii Torr. dry powder in S1 and add the distilled water of described Salicornia Bigelovii Torr. dry powder weight 15 times, tune pH value is
5.5, add 0.03% compound enzyme (ratio of cellulase, hemicellulase and pectase is 1:1:0.7) and 200mpa's
Enzymolysis 20min under the conditions of vacuum tightness, and hydrolysis temperature controls at 48 DEG C, through homogenate extraction, (extraction time 1.5min extracts
Temperature 35 DEG C, extracts voltage 120V), it is centrifuged, is filtrated to get supernatant a and filtering residue;
S3. the supernatant a taking S2 gained concentrates, and then adds the extract (chloroform) of concentrated solution volume 2 times, stir,
Stand, be extracted liquid layer and supernatant layer, be isolated to supernatant b;
S4. the supernatant b obtained by S3 concentrates, and then adds the second that volumetric concentration is 70% of concentrated solution volume 8 times
Alcohol, extracts 2h, is centrifuged, is filtrated to get supernatant b and deposit, then supernatant c concentration, lyophilization is obtained total flavones
Crude product;
S5. the total flavones crude product obtained by S4, dissolves with distilled water, then crosses macroporous resin column (D101-B), and uses body
Volume concentrations be 65% ethanol it is carried out eluting, eluent flow rate 1.5ml/min, collect eluent, then that eluent is dense
Contracting, lyophilization obtain refined total flavonoids;
S6. the deposit distilled water obtained by S4 dissolves, and is subsequently adding the Fructus Chaenomelis egg of deposit weight 0.15%
White enzyme, and adjust pH value of solution for neutrality, hydrolyzes 1h under the conditions of 65 DEG C, enzyme denaturing, dialyses 24h with tap water, uses distilled water the most again
Dialysis 12h, concentrates, obtains refined polysaccharide after drying.
Wherein when operating S3 step, take the filtering residue that S2 obtains, then with 60% ethanol, homogenate extraction, extraction time
1.5min, Extracting temperature 30 DEG C, to extract voltage 120V and be centrifuged, filter, the filtrate obtained merges with described supernatant a.
Under these process conditions, in Salicornia Bigelovii Torr., total flavones extraction ratio is 258mg/g, and purity is 85.6%;The extraction ratio of polysaccharide
52.6mg/g, purity is 86.3%.
Example 3
A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method thereof, comprise the following steps:
S1. pluck the fresh leaf of Salicornia Bigelovii Torr., through over cleaning, be dried, pulverized 60 mesh sieves, obtain Salicornia Bigelovii Torr. dry powder;
S2. weighing the Salicornia Bigelovii Torr. dry powder in S1 and add the distilled water of described Salicornia Bigelovii Torr. dry powder weight 12 times, tune pH value is
5.5, add 0.04% compound enzyme (ratio of cellulase, hemicellulase and pectase is 1.1:0.8:0.7) and
Enzymolysis 22min under the conditions of the vacuum tightness of 240mpa, and hydrolysis temperature controls at 60 DEG C, through homogenate extraction (extraction time
1min, Extracting temperature 36 DEG C, extract voltage 130V), it is centrifuged, is filtrated to get supernatant a and filtering residue;
S3. the supernatant a taking S2 gained concentrates, and then adds the extract of concentrated solution volume 2.5 times, stirs, stands,
It is extracted liquid layer and supernatant layer, is isolated to supernatant b;
S4. the supernatant b obtained by S3 concentrates, and then adds the second that volumetric concentration is 70% of concentrated solution volume 6 times
Alcohol, extracts 2.5h, is centrifuged, is filtrated to get supernatant b and deposit, then supernatant c concentration, lyophilization is obtained total Huang
Ketone crude product;
S5. the total flavones crude product obtained by S4, dissolves with distilled water, then crosses macroporous resin column (AB-8), and uses volume
Concentration be 70% ethanol it is carried out eluting, eluent flow rate 1.5ml/min, collect eluent, then eluent is concentrated,
Lyophilization obtains Refined flavonoid powder;
S6. the deposit distilled water obtained by S4 dissolves, and is subsequently adding the Fructus Chaenomelis of many deposits weight 0.17%
Protease, and adjust pH value of solution for neutrality, hydrolyze 0.5h, enzyme denaturing under the conditions of 70 DEG C, dialyse 24h with tap water, the most again with steaming
Distilled water dialysis 12h, concentrates, obtains refined polysaccharide after drying.
Under these process conditions, in Salicornia Bigelovii Torr., total flavones extraction ratio is 243mg/g, and purity is 83.2%;The extraction ratio of polysaccharide
48.6mg/g, purity is 84.8%.
Example 4
A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method thereof, comprise the following steps:
S1. pluck the fresh leaf of Salicornia Bigelovii Torr., through over cleaning, be dried, pulverized 80 mesh sieves, obtain Salicornia Bigelovii Torr. dry powder;
S2. weighing the Salicornia Bigelovii Torr. dry powder in S1 and add the distilled water of described Salicornia Bigelovii Torr. dry powder weight 18 times, tune pH value is
5.8, add 0.05% compound enzyme (ratio of cellulase, hemicellulase and pectase is 1.3:0.7:0.7) and
Enzymolysis 15min under the conditions of the vacuum tightness of 300mpa, and hydrolysis temperature controls at 45 DEG C, through homogenate extraction (extraction time
1min, Extracting temperature 42 DEG C, extract voltage 140V), it is centrifuged, is filtrated to get supernatant a and filtering residue;
S3. the supernatant a taking S2 gained concentrates, and then adds the extract of concentrated solution volume 3 times, stirs, stands,
To extraction liquid layer and supernatant layer, it is isolated to supernatant b;
S4. the supernatant b obtained by S3 concentrates, and then adds the second that volumetric concentration is 75% of concentrated solution volume 10 times
Alcohol, extracts 3h, is centrifuged, is filtrated to get supernatant b and deposit, then supernatant c concentration, lyophilization is obtained total flavones
Crude product;
S5. the total flavones crude product obtained by S4, dissolves with distilled water, then crosses macroporous resin column (D101-B), and uses body
Volume concentrations is that 65% ethanol carries out eluting, eluent flow rate 1.8ml/min to it, collects eluent, then eluent is concentrated,
Lyophilization obtains Refined flavonoid powder;
S6. the deposit distilled water obtained by S4 dissolves, and is subsequently adding the Papain of deposit weight 0.2%
Enzyme, and adjust pH value of solution for neutrality, hydrolyze 0.5h, enzyme denaturing under the conditions of 68 DEG C, dialyse 24h with tap water, use distilled water the most again
Dialysis 12h, concentrates, obtains refined polysaccharide after drying.
Under these process conditions, in Salicornia Bigelovii Torr., total flavones extraction ratio is 252mg/g, and purity is 84.2%;The extraction ratio of polysaccharide
50.6mg/g, purity is 85.7%.
The present invention uses enzymolysis solution effectively to degrade the cell wall constituent of Salicornia Bigelovii Torr. under elevated pressure conditions, then in conjunction with
Homogenate extraction method, makes the total flavones in Salicornia Bigelovii Torr. and polysaccharide discharge from cell wall, and is transferred quickly in Extraction solvent, carry
The time that takes is short, the most also improve total flavones extraction ratio, then by the extraction of organic solvent, removes pigment, alcohol steep, macropore
Resin isolated and purified, enzyme process removing protein, dialysis remove salinity and small-molecule substance so that respectively obtain refined total flavonoids and
Refined polysaccharide.The method technique is simple, and easy to operate, feasibility is good.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (10)
1. a Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method, it is characterised in that described extracting method comprises the following steps:
S1. pluck the fresh leaf of Salicornia Bigelovii Torr., through over cleaning, dry, pulverizing, obtain Salicornia Bigelovii Torr. dry powder;
S2. weigh the Salicornia Bigelovii Torr. dry powder in S1 and add the distilled water of described Salicornia Bigelovii Torr. dry powder weight 10-18 times, adjusting pH value to exist
Between 4.8-6, addition compound enzyme enzymolysis 15-25min under the conditions of the vacuum tightness of 100-200mpa, through homogenate extraction
After, it is centrifuged, is filtrated to get supernatant a and filtering residue;
S3. the supernatant a taking S2 gained concentrates, and then adds the extract of concentrated solution volume 1-3 times, stirs, stands, obtain
Extraction liquid layer and supernatant layer, be isolated to supernatant b;
S4. the supernatant b obtained by S3 concentrates, and the volumetric concentration then adding concentrated solution volume 6-10 times is 60%-80%
Ethanol, extract 1-3h, be centrifuged, be filtrated to get supernatant c and deposit, then supernatant c is concentrated, lyophilization obtains
Total flavones crude product;
S5. the total flavones crude product obtained by S4, dissolves with distilled water, then crosses macroporous resin column, and is 50%-by volumetric concentration
The ethanol of 75% carries out eluting to it, collects eluent, then eluent concentration, lyophilization is obtained Refined flavonoid powder;
S6. the deposit distilled water obtained by S4 dissolves, and is subsequently adding the Papain of deposit weight 0.1-0.2%
Enzyme, and adjust pH value of solution for neutrality, under the conditions of 60-70 DEG C hydrolyze 0.5-1h, enzyme denaturing, dialyse, concentrate, refined after drying many
Sugar.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described sudden strain of a muscle
Formula extraction conditions: extraction time 0.5-2min, Extracting temperature 25-45 DEG C, extracts voltage 110-150V.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described multiple
The addition of synthase is the 0.02%-0.05% of described Salicornia Bigelovii Torr. dry powder weight.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described multiple
Synthase is cellulase, hemicellulase and pectase, and the ratio of described cellulase, hemicellulase and pectase is
0.6-1.3:0.7-1:0.5-0.7。
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described enzyme
The hydrolysis temperature solved is 40-65 DEG C.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: take S2 and obtain
The filtering residue arrived, then with 60% ethanol, homogenate extraction, centrifugal, filter, the filtrate obtained merges with described supernatant a.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described S4
In the concentration of ethanol be 70%.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described S5
Middle macroporous resin column selects AB-8, HPD-722 or D101-B.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 1 and polysaccharide combined extraction method, it is characterised in that: described S3
In extract be petroleum ether, chloroform, normal hexane or ethyl acetate.
A kind of Salicornia Bigelovii Torr. total flavones the most according to claim 9 and polysaccharide combined extraction method, it is characterised in that: described
Extract in S3 is chloroform.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610624969.5A CN106220748B (en) | 2016-07-30 | 2016-07-30 | A kind of sea asparagus general flavone and polysaccharide combined extraction method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610624969.5A CN106220748B (en) | 2016-07-30 | 2016-07-30 | A kind of sea asparagus general flavone and polysaccharide combined extraction method |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106220748A true CN106220748A (en) | 2016-12-14 |
CN106220748B CN106220748B (en) | 2018-07-06 |
Family
ID=57536407
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610624969.5A Active CN106220748B (en) | 2016-07-30 | 2016-07-30 | A kind of sea asparagus general flavone and polysaccharide combined extraction method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106220748B (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109880864A (en) * | 2019-03-06 | 2019-06-14 | 福州大学 | The enzyme process method for integrated extraction of function polysaccharide and procyanidine in a kind of longan peel |
CN112142866A (en) * | 2020-08-28 | 2020-12-29 | 盐城工学院 | Extraction method of froggrass polysaccharide with blood sugar reducing effect |
CN113785979A (en) * | 2021-09-10 | 2021-12-14 | 宝得瑞(湖北)健康产业有限公司 | Instant asparagus powder with high saponin content and low potassium content and preparation method thereof |
CN114524886A (en) * | 2022-03-10 | 2022-05-24 | 广西中医药大学 | Non-starch elemi total polysaccharide, preparation method thereof and application of non-starch elemi total polysaccharide as intestinal prebiotics |
CN114668143A (en) * | 2022-04-24 | 2022-06-28 | 麻城市正旺芦笋农业科技股份有限公司 | Method for extracting and separating nutrient components of asparagus |
CN115197335A (en) * | 2022-05-12 | 2022-10-18 | 上海应用技术大学 | Yam polysaccharide and extraction method and application thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101967137A (en) * | 2010-09-21 | 2011-02-09 | 天津市食品加工工程中心 | Method for extracting plant flavone compounds by enzymatic process |
CN102940688A (en) * | 2012-10-15 | 2013-02-27 | 威海新异生物科技有限公司 | Extraction method for polysaccharides and total flavonoids in fig leaves |
CN103432196A (en) * | 2012-12-06 | 2013-12-11 | 重庆科瑞制药(集团)有限公司 | Desmodium styracifolium total flavonoids and preparation method of Desmodium styracifolium total flavonoids and total polysaccharides |
CN105567409A (en) * | 2015-12-22 | 2016-05-11 | 福建农林大学 | Method using flash-assisting composite enzymatic hydrolysis to extract tea seed oil |
-
2016
- 2016-07-30 CN CN201610624969.5A patent/CN106220748B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101967137A (en) * | 2010-09-21 | 2011-02-09 | 天津市食品加工工程中心 | Method for extracting plant flavone compounds by enzymatic process |
CN102940688A (en) * | 2012-10-15 | 2013-02-27 | 威海新异生物科技有限公司 | Extraction method for polysaccharides and total flavonoids in fig leaves |
CN103432196A (en) * | 2012-12-06 | 2013-12-11 | 重庆科瑞制药(集团)有限公司 | Desmodium styracifolium total flavonoids and preparation method of Desmodium styracifolium total flavonoids and total polysaccharides |
CN105567409A (en) * | 2015-12-22 | 2016-05-11 | 福建农林大学 | Method using flash-assisting composite enzymatic hydrolysis to extract tea seed oil |
Non-Patent Citations (2)
Title |
---|
扶庆权等: ""微波辅助提取海蓬子总黄酮工艺的响应曲面法优化"", 《南京师大学报(自然科学版)》 * |
管福琴等: ""海蓬子属植物药理活性及其作用机制研究进展"", 《中国药理学通报》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109880864A (en) * | 2019-03-06 | 2019-06-14 | 福州大学 | The enzyme process method for integrated extraction of function polysaccharide and procyanidine in a kind of longan peel |
CN112142866A (en) * | 2020-08-28 | 2020-12-29 | 盐城工学院 | Extraction method of froggrass polysaccharide with blood sugar reducing effect |
CN113785979A (en) * | 2021-09-10 | 2021-12-14 | 宝得瑞(湖北)健康产业有限公司 | Instant asparagus powder with high saponin content and low potassium content and preparation method thereof |
CN114524886A (en) * | 2022-03-10 | 2022-05-24 | 广西中医药大学 | Non-starch elemi total polysaccharide, preparation method thereof and application of non-starch elemi total polysaccharide as intestinal prebiotics |
CN114668143A (en) * | 2022-04-24 | 2022-06-28 | 麻城市正旺芦笋农业科技股份有限公司 | Method for extracting and separating nutrient components of asparagus |
CN115197335A (en) * | 2022-05-12 | 2022-10-18 | 上海应用技术大学 | Yam polysaccharide and extraction method and application thereof |
Also Published As
Publication number | Publication date |
---|---|
CN106220748B (en) | 2018-07-06 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106220748A (en) | A kind of Salicornia Bigelovii Torr. total flavones and polysaccharide combined extraction method | |
US20220080333A1 (en) | Ultrasonic composite acidic water extraction method for cordyceps polysaccharide and cordycepin in cordyceps militaris | |
CN103864949A (en) | Method for preparing maca polysaccharide and maca alkaloid by use of membrane separation technique | |
CN106046192A (en) | Process for extracting pachyman from poria coccus wolf | |
CN106381319A (en) | High-efficiency extraction and separation method of grape seed proanthocyanidin oligomer | |
CN104045724B (en) | The method that Fuscoporia obliqua polysaccharide is prepared in extraction from Inonqqus obliquus | |
CN106213523A (en) | A kind of extracting method of Salicornia Bigelovii Torr. dietary fiber | |
CN102453601B (en) | Extraction method of Cinnamomum camphora seed oil by ultrasound-assisted compound enzyme | |
CN106832030A (en) | The method that active polysaccharide is extracted from marine alga | |
CN106478578A (en) | A kind of method of physical field assisted extraction Exocarpium Litchi procyanidin | |
CN103519180A (en) | Preparation method of maca extract | |
CN104961839A (en) | Preparation method of specific pachyman formula granule | |
CN106109515A (en) | A kind of extracting method of total Flavonoids from Suaeda salsa | |
CN108210555A (en) | A kind of homogenate extraction method of glycyrrhiza total flavonoid | |
CN104531822B (en) | A kind of purple sweet potato cyanidin efficiently synthesizes extracting method | |
CN104592412A (en) | Method for extracting chestnut polysaccharide | |
CN102630943A (en) | Spirulina gamma-linolenic acid extractive and preparation method thereof | |
CN110592167B (en) | Purslane polypeptide extract and preparation method thereof | |
CN105367433A (en) | Method for extracting gamma-aminobutyric acid from barley germs | |
CN102408400A (en) | Method for co-production of wheat germ flavone, raffinose and wheat germ concentrated protein by taking degreased wheat germ as raw material | |
CN105566507A (en) | Preparation method of tea polysaccharides | |
CN105266075B (en) | method for extracting Stichopus japonicus saponins from Stichopus japonicus blanching liquid | |
CN103725740A (en) | Method for extracting glycoprotein by using scollop blanching liquid | |
US8092842B2 (en) | Extraction of phytochemicals by enzymatic hydrolysis | |
CN107903328A (en) | A kind of wrinkled papaya seed polysaccharide and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
CB02 | Change of applicant information | ||
CB02 | Change of applicant information |
Address after: 261108 00800 Xiang Jiangxi street, Binhai Economic Development Zone, Weifang, Shandong Applicant after: Shandong Sheng Wei salt alkali land Technology Co., Ltd. Address before: 261108 00800 Xiang Jiangxi street, Binhai Economic Development Zone, Weifang, Shandong Applicant before: Shandong Sunway Garden Technology Co., Ltd. |
|
GR01 | Patent grant | ||
GR01 | Patent grant |