CN106220748B - A kind of sea asparagus general flavone and polysaccharide combined extraction method - Google Patents
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Abstract
Extraction more particularly to a kind of extra large asparagus general flavone and polysaccharide combined extraction method the present invention relates to active components of plants, include the following steps：S1. extra large asparagus, cleaning, dry, crushing, sieving, obtains extra large asparagus dry powder；S2. it weighs dry powder and adds in distilled water, adjust pH value, digested under the conditions of addition complex enzyme vacuum tightness, extract, centrifuge, supernatant a and filter residue is obtained by filtration；S3. supernatant a is taken to concentrate, extract liquor extraction detaches to obtain supernatant b；S4. supernatant b is concentrated, adds ethyl alcohol, extracted, centrifuge, supernatant c and deposit is obtained by filtration, by concentrating, being dried to obtain general flavone crude product；S5. it is adsorbed by macroporous resin column, ethanol elution, collects 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, easy to operate, and the time is short, and effectively removes chlorophyll, salinity and other miscellaneous point, improves the yield and product purity of general flavone and polysaccharide.
Description
Technical field
Extraction more particularly to a kind of extra large asparagus general flavone and polysaccharide synthesis extraction side the present invention relates to active components of plants
Method.
Background technology
Extra large asparagus (Salicornia) is the euhalophyte without base of leaf carnification that Chenopodiaceae salicornia europaeal belongs to, and the tolerance of salinity is high,
Marine borer grass, salicornia europaeal, extra large covering or extra large beans are commonly called as, are more common in lick, seabeach is taken up in salt lake.Recently as both at home and abroad to sea
Asparagus research deepens continuously, and isolated polysaccharide, chromocor compound, biogenic salt, chlorophyll etc. are a variety of from extra large asparagus
Active constituent with medical value and health value.By research shows that chromocor compound has softening blood vessel, hypoglycemic, drop
Blood fat, anti-oxidant, removing interior free yl, anti-aging, resisting pathogenic microbes, anti-infective, anti-inflammatory, antiulcer, antiallergy, rush
Into different physiological roles such as regenerations；There is polysaccharide antitumor, antiviral, antiulcer, radioresistance, enhancing to be immunized, is antifatigue
And other effects.
Chromocor compound is extracted from extra large asparagus at present, is generally extracted using organic solvent method or microwave radiation technology organic solvent
Method, by decolourizing, isolating and purifying, being dried to obtain flavones product.But using above method extraction chromocor compound, there are some
Problem：Extraction time is long, post processing extraction solvent consumption is big, and chromocor compound is surrounded by the cell wall based on cellulose, and
Iuntercellular has pectin bonding, can hinder solute mass transfer in extraction process, causes chromocor compound recovery rate low, chromocor compound production
Product purity is low.Although the prior art also has extracts flavonoid substance using using enzymatic isolation method from other raw materials, using enzymolysis
When method extracts flavones, enzymolysis time is long, reaction time consumption, and recovery rate is low.
There are many extracting methods of polysaccharide, extracts polysaccharide material from extra large asparagus at present, is generally carried using ultrasonic wave auxiliary
It follows the example of, is analysed by alcohol, the links such as de- albumen, dialysis, drying obtain polyose.Although it is generated using ultra sonic machinery vibration
Energy makes medium structure change, active ingredient is promoted to rapidly enter in solvent to a certain extent, but plant cell wall
Structure comparatively robust, the recovery rate of polysaccharide material is low, when current polysaccharide takes off albumen in addition, generally using Sevage methods, TCA methods and
NaOH methods can all cause the loss of polysaccharide component.Therefore the present invention is based on the prior arts to extract problem present in flavones and polysaccharide,
Establish a kind of extra large asparagus general flavone and polysaccharide combined extraction method.
Invention content
The technical problems to be solved by the invention are：In view of the deficienciess of the prior art, provide a kind of extra large Asparagus Flavonoids
And polysaccharide combined extraction method, the method is simple for process, easy to operate, and the time is short, while can improve chromocor compound, polysaccharide material again
The recovery rate and purity of matter.
In order to solve the above technical problems, the technical scheme is that：
A kind of sea asparagus general flavone and polysaccharide combined extraction method, the extracting method include the following steps：
S1. extra large asparagus fresh leaf is picked, through over cleaning, drying, crushing, obtains extra large asparagus dry powder；
S2. it weighs the extra large asparagus dry powder in S1 and adds in the distilled water of extra large 10-18 times of the asparagus dry powder weight, adjust pH value
Between 4.8-6, add in complex enzyme and digest 15-25min under the conditions of the vacuum tightness of 100-200mpa, by homogenate extraction
Afterwards, it centrifuges, supernatant a and filter residue is obtained by filtration；
S3. the supernatant a obtained by S2 is taken to concentrate, then adds the extract liquor of 1-3 times of the volume of the concentrated liquid, stirring is stood,
Extraction liquid layer and supernatant layer are obtained, is isolated to supernatant b；
S4. supernatant b S3 obtained is concentrated, and the volumetric concentration for then adding 6-10 times of the volume of the concentrated liquid is 60%-
80% ethyl alcohol extracts 1-3h, centrifuges, supernatant c and deposit is obtained by filtration, then by supernatant c concentrations, freeze-drying
Obtain general flavone crude product；
S5. general flavone crude product S4 obtained with distillation water dissolution, then crosses macroporous resin column, and be with volumetric concentration
The ethyl alcohol of 50%-75% elutes it, collects eluent, then concentrates eluent, is freeze-dried and obtains Refined flavonoid powder；
S6. by the deposit that S4 is obtained distillation water dissolution, the pawpaw of deposit weight 0.1-0.2% is then added in
Protease, and pH value of solution is adjusted as neutrality, 0.5-1h is hydrolyzed under the conditions of 60-70 DEG C, essence is obtained after enzyme deactivation, dialysis, concentration, drying
Polysaccharide processed.
As an improvement technical solution, the homogenate extraction condition：Extraction time 0.5-2min, Extracting temperature 25-
45 DEG C, extraction voltage 110-150V.
As a kind of perferred technical scheme, the addition of the complex enzyme is the extra large asparagus dry powder weight
0.02%-0.05%.
As an improvement technical solution, the complex 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 a kind of perferred technical scheme, the hydrolysis temperature of the enzymolysis is 40-65 DEG C.
As an improvement technical solution, the filter residue that S2 is taken to obtain, then with 60% ethyl alcohol, homogenate extraction, centrifugation,
Filtering, obtained filtrate merge with the supernatant a.
As a kind of perferred technical scheme, a concentration of 70% of the ethyl alcohol in the S4.
As a kind of perferred technical scheme, macroporous resin column selects AB-8, HPD-722 or D101-B in the S5.
As a kind of perferred technical scheme, the extract liquor in the S3 is petroleum ether, chloroform, n-hexane or acetic acid second
Ester.
As a kind of further preferred technical solution, the extract liquor in the S3 is chloroform.
After employing above-mentioned technical proposal, the beneficial effects of the invention are as follows：
Compared with prior art, the present invention mainly has the following advantages：
(1) extra large asparagus is digested under confined conditions in high pressure vacuum using complex enzyme, enzymolysis time can be shortened, simultaneously
Enzymolysis liquid and Extraction solvent quickly entered in boosting in vascular bundle and gland cell, make inside extra large asparagus flavones in cell wall and
Polysaccharide releases completely, then active ingredient can be made to be quickly transferred in Extraction solvent using homogenate extraction, and extraction time is short,
The recovery rate of general flavone is improved simultaneously, and extracting flavonoids rate can be made to reach 258mg/g；By macroporous resin column to chromocor compound
It is enriched with, elution further detaches flavones crude product, purifies, and improves the purity of chromocor compound, and purify
The flavones content of extra large asparagus reaches 85.6% in extract afterwards；
(2) chlorophyll can effectively be removed by extract liquor extraction, removes and desalt through alcohol steep, protease removing protein, dialysis
Grade small-molecule substance, can obtain refined polysaccharide, and polysaccharide extract rate reaches 52.6mg/g, and purity reaches 86.3%；
(3) present invention takes full advantage of extra large asparagus resource, realizes the extraction to polysaccharide, technique letter while extracting flavones again
It is single, easy to operate, organic solvent toxicity is small, it is easy recycling, feasibility it is good.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Example 1
A kind of sea asparagus general flavone and its polysaccharide combined extraction method, include the following steps：
S1. extra large asparagus fresh leaf is picked, through over cleaning, drying, 20 mesh sieve is crushed, obtains extra large asparagus dry powder；
S2. it weighs the extra large asparagus dry powder in S1 and adds in the distilled water of extra large 10 times of the asparagus dry powder weight, tune pH value is
4.8, adding in 0.02% complex enzyme, (ratio of cellulase, hemicellulase and pectase is 0.6:1:0.7) and in 100mpa
Vacuum tightness under the conditions of digest 25min, and hydrolysis temperature control, at 40 DEG C, (extraction time 0.5min, carries by homogenate extraction
30 DEG C of temperature is taken, extracts voltage 110V), it centrifuges, supernatant a and filter residue is obtained by filtration；
S3. the supernatant a obtained by S2 is taken to concentrate, the extract liquor (petroleum ether) of 1.5 times of the volume of the concentrated liquid is then added, stirs
It mixes, stand, obtain extraction liquid layer and supernatant layer, be isolated to supernatant b；
S4. supernatant b S3 obtained is concentrated, and the volumetric concentration for then adding 6 times of the volume of the concentrated liquid is 60% second
Alcohol extracts 1.5h, centrifuges, supernatant b and deposit is obtained by filtration, and supernatant c concentrations, freeze-drying then are obtained total Huang
Ketone crude product；
S5. general flavone crude product S4 obtained with distillation water dissolution, then crosses macroporous resin column (HPD-722), first with steaming
Distilled water elutes, and then it is eluted with the ethyl alcohol that volumetric concentration is 60%, eluent flow rate 1ml/min, collects ethyl alcohol and washes
Then eluent is concentrated, is freeze-dried and obtains refined total flavonoids by the eluent flowed out when de-；
S6. by the deposit that S4 is obtained distillation water dissolution, the Papain of deposit weight 0.1% is then added in
Enzyme, and pH value of solution is adjusted as neutrality, 0.5h is hydrolyzed under the conditions of 60 DEG C, enzyme deactivation with tap water dialysis for 24 hours, then uses distilled water again
Dialyse 12h, and refined polysaccharide is obtained after concentration, drying.
General flavone recovery rate is 239mg/g in extra large asparagus under this process condition, purity 82.9%；The recovery rate of polysaccharide
43.5mg/g, purity 82.4%.
Example 2
A kind of sea asparagus general flavone and its polysaccharide combined extraction method, include the following steps：
S1. extra large asparagus fresh leaf is picked, through over cleaning, drying, 40 mesh sieve is crushed, obtains extra large asparagus dry powder；
S2. it weighs the extra large asparagus dry powder in S1 and adds in the distilled water of extra large 15 times of the asparagus dry powder weight, tune pH value is
5.5, adding in 0.03% complex enzyme, (ratio of cellulase, hemicellulase and pectase is 1:1:0.7) and 200mpa's
20min is digested under the conditions of vacuum tightness, and hydrolysis temperature control, at 48 DEG C, (extraction time 1.5min is extracted by homogenate extraction
35 DEG C of temperature extracts voltage 120V), it centrifuges, supernatant a and filter residue is obtained by filtration；
S3. the supernatant a obtained by S2 is taken to concentrate, then adds the extract liquor (chloroform) of 2 times of the volume of the concentrated liquid, stir,
It stands, obtains extraction liquid layer and supernatant layer, be isolated to supernatant b；
S4. supernatant b S3 obtained is concentrated, and the volumetric concentration for then adding 8 times of the volume of the concentrated liquid is 70% second
Alcohol extracts 2h, centrifuges, supernatant b and deposit is obtained by filtration, and supernatant c concentrations, freeze-drying then are obtained general flavone
Crude product；
S5. general flavone crude product S4 obtained with distillation water dissolution, then crosses macroporous resin column (D101-B), and use body
The ethyl alcohol of product a concentration of 65% elutes it, eluent flow rate 1.5ml/min, collects eluent, then that eluent is dense
Contracting, freeze-drying obtain refined total flavonoids；
S6. by the deposit that S4 is obtained distillation water dissolution, the pawpaw egg of deposit weight 0.15% is then added in
White enzyme, and pH value of solution is adjusted as neutrality, 1h is hydrolyzed under the conditions of 65 DEG C, enzyme deactivation with tap water dialysis for 24 hours, then uses distilled water again
Dialyse 12h, and refined polysaccharide is obtained after concentration, drying.
Wherein when operating S3 steps, filter residue that S2 is taken to obtain, then with 60% ethyl alcohol, homogenate extraction, extraction time
1.5min, 30 DEG C of Extracting temperature, extraction voltage 120V centrifugations, filtering, obtained filtrate merge with the supernatant a.
General flavone recovery rate is 258mg/g in extra large asparagus under this process condition, purity 85.6%；The recovery rate of polysaccharide
52.6mg/g, purity 86.3%.
Example 3
A kind of sea asparagus general flavone and its polysaccharide combined extraction method, include the following steps：
S1. extra large asparagus fresh leaf is picked, through over cleaning, drying, 60 mesh sieve is crushed, obtains extra large asparagus dry powder；
S2. it weighs the extra large asparagus dry powder in S1 and adds in the distilled water of extra large 12 times of the asparagus dry powder weight, tune pH value is
5.5, adding in 0.04% complex enzyme, (ratio of cellulase, hemicellulase and pectase is 1.1:0.8:0.7) and
22min is digested under the conditions of the vacuum tightness of 240mpa, and hydrolysis temperature is controlled at 60 DEG C, by homogenate extraction (extraction time
1min, 36 DEG C of Extracting temperature extract voltage 130V), it centrifuges, supernatant a and filter residue is obtained by filtration；
S3. the supernatant a obtained by S2 is taken to concentrate, then adds the extract liquor of 2.5 times of the volume of the concentrated liquid, stirring is stood,
Extraction liquid layer and supernatant layer are obtained, is isolated to supernatant b；
S4. supernatant b S3 obtained is concentrated, and the volumetric concentration for then adding 6 times of the volume of the concentrated liquid is 70% second
Alcohol extracts 2.5h, centrifuges, supernatant b and deposit is obtained by filtration, and supernatant c concentrations, freeze-drying then are obtained total Huang
Ketone crude product；
S5. general flavone crude product S4 obtained with distillation water dissolution, then crosses macroporous resin column (AB-8), and use volume
A concentration of 70% ethyl alcohol elutes it, eluent flow rate 1.5ml/min, collects eluent, then concentrate eluent,
Freeze-drying obtains Refined flavonoid powder；
S6. by the deposit that S4 is obtained distillation water dissolution, the pawpaw of more deposit weight 0.17% is then added in
Protease, and pH value of solution is adjusted as neutrality, 0.5h, enzyme deactivation, with tap water dialysis for 24 hours, then again with steaming are hydrolyzed under the conditions of 70 DEG C
Distilled water dialysis 12h, refined polysaccharide is obtained after concentration, drying.
General flavone recovery rate is 243mg/g in extra large asparagus under this process condition, purity 83.2%；The recovery rate of polysaccharide
48.6mg/g, purity 84.8%.
Example 4
A kind of sea asparagus general flavone and its polysaccharide combined extraction method, include the following steps：
S1. extra large asparagus fresh leaf is picked, through over cleaning, drying, 80 mesh sieve is crushed, obtains extra large asparagus dry powder；
S2. it weighs the extra large asparagus dry powder in S1 and adds in the distilled water of extra large 18 times of the asparagus dry powder weight, tune pH value is
5.8, adding in 0.05% complex enzyme, (ratio of cellulase, hemicellulase and pectase is 1.3:0.7:0.7) and
15min is digested under the conditions of the vacuum tightness of 300mpa, and hydrolysis temperature is controlled at 45 DEG C, by homogenate extraction (extraction time
1min, 42 DEG C of Extracting temperature extract voltage 140V), it centrifuges, supernatant a and filter residue is obtained by filtration；
S3. the supernatant a obtained by S2 is taken to concentrate, then adds the extract liquor of 3 times of the volume of the concentrated liquid, stirring is stood, and is obtained
To extraction liquid layer and supernatant layer, it is isolated to supernatant b；
S4. supernatant b S3 obtained is concentrated, and the volumetric concentration for then adding 10 times of the volume of the concentrated liquid is 75% second
Alcohol extracts 3h, centrifuges, supernatant b and deposit is obtained by filtration, and supernatant c concentrations, freeze-drying then are obtained general flavone
Crude product；
S5. general flavone crude product S4 obtained with distillation water dissolution, then crosses macroporous resin column (D101-B), and use body
A concentration of 65% ethyl alcohol of product elutes it, and eluent flow rate 1.8ml/min collects eluent, then concentrate eluent,
Freeze-drying obtains Refined flavonoid powder；
S6. by the deposit that S4 is obtained distillation water dissolution, the Papain of deposit weight 0.2% is then added in
Enzyme, and pH value of solution is adjusted as neutrality, 0.5h is hydrolyzed under the conditions of 68 DEG C, enzyme deactivation with tap water dialysis for 24 hours, then uses distilled water again
Dialyse 12h, and refined polysaccharide is obtained after concentration, drying.
General flavone recovery rate is 252mg/g in extra large asparagus under this process condition, purity 84.2%；The recovery rate of polysaccharide
50.6mg/g, purity 85.7%.
The present invention under high pressure effectively degrades to the cell wall constituent of extra large asparagus using enzymolysis liquid, then in conjunction with
Homogenate extraction method makes general flavone and polysaccharide in extra large asparagus be released from cell wall, and be transferred quickly in Extraction solvent, carries
It takes the time short while also improves general flavone recovery rate, then by the extraction of organic solvent, remove pigment, alcohol steep, macropore
Resin isolates and purifies, enzyme process removing protein, dialysis remove salinity and small-molecule substance so that respectively obtain refined total flavonoids and
Refined polysaccharide.This method is simple for process, easy to operate, and feasibility is good.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of sea asparagus general flavone and polysaccharide combined extraction method, it is characterised in that the extracting method includes the following steps：
S1. extra large asparagus fresh leaf is picked, through over cleaning, drying, crushing, obtains extra large asparagus dry powder；
S2. it weighs the extra large asparagus dry powder in S1 and adds in the distilled water of extra large 10-18 times of the asparagus dry powder weight, pH value is adjusted to exist
Between 4.8-6, add in by cellulase, hemicellulase and pectase according to 0.6-1.3：0.7-1：The ratio group of 0.5-0.7
Into complex enzyme and digest 15-25min under the conditions of the vacuum tightness of 100-200mPa, after homogenate extraction, centrifugation, mistake
Filter obtains supernatant a and filter residue；
S3. the supernatant a obtained by S2 is taken to concentrate, then adds the extract liquor of 1-3 times of the volume of the concentrated liquid, stirring is stood, and is obtained
Liquid layer and supernatant layer are extracted, is isolated to supernatant b；
S4. supernatant b S3 obtained is concentrated, and the volumetric concentration for then adding 6-10 times of the volume of the concentrated liquid is 60%-80%
Ethyl alcohol, extract 1-3h, centrifuge, supernatant c and deposit be obtained by filtration, then by supernatant c concentration, freeze-drying obtain
General flavone crude product；
S5. general flavone crude product S4 obtained with distillation water dissolution, then crosses macroporous resin column, and be 50%- with volumetric concentration
75% ethyl alcohol elutes it, collects eluent, then concentrates eluent, is freeze-dried and obtains Refined flavonoid powder；
S6. by the deposit that S4 is obtained distillation water dissolution, the Papain of deposit weight 0.1-0.2% is then added in
Enzyme, and pH value of solution is adjusted as neutrality, 0.5-1h is hydrolyzed under the conditions of 60-70 DEG C, is obtained after enzyme deactivation, dialysis, concentration, drying refined more
Sugar.
2. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：The sudden strain of a muscle
Formula extraction conditions：Extraction time 0.5-2min, 25-45 DEG C of Extracting temperature, extraction voltage 110-150V.
3. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：It is described multiple
0.02%-0.05% of the addition of synthase for the extra large asparagus dry powder weight.
4. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：The enzyme
The hydrolysis temperature of solution is 40-65 DEG C.
5. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：S2 is taken to obtain
The filter residue arrived, then with 60% ethyl alcohol, homogenate extraction, centrifugation, filtering, obtained filtrate merges with the supernatant a.
6. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：The S4
In ethyl alcohol a concentration of 70%.
7. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：The S5
Middle macroporous resin column selects AB-8, HPD-722 or D101-B.
8. a kind of extra large asparagus general flavone according to claim 1 and polysaccharide combined extraction method, it is characterised in that：The S3
In extract liquor be petroleum ether, chloroform, n-hexane or ethyl acetate.
9. a kind of extra large asparagus general flavone according to claim 8 and polysaccharide combined extraction method, it is characterised in that：The S3
In extract liquor be chloroform.
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