CN107118102B - A method of preparing leaf of bamboo polyphenol from the leaf of bamboo - Google Patents
A method of preparing leaf of bamboo polyphenol from the leaf of bamboo Download PDFInfo
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- CN107118102B CN107118102B CN201710246445.1A CN201710246445A CN107118102B CN 107118102 B CN107118102 B CN 107118102B CN 201710246445 A CN201710246445 A CN 201710246445A CN 107118102 B CN107118102 B CN 107118102B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
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Abstract
The present invention relates to leaf of bamboo extracts, and in particular to the method for leaf of bamboo polyphenol is prepared from the leaf of bamboo.This method comprises the steps of: (1) taking leaf of bamboo powder that ethanol solution, ultrasonic extraction is added by the solid-to-liquid ratio of 1g: 10~20mL, membrane filtration obtains crude extract;(2) zirconium oxide is added into crude extract in the ratio that 0.2~0.5g zirconium oxide is added in 1mL crude extract, shaking table vibrates 1~4 hour, is centrifugated out zirconium oxide ethanol washing;(3) is added 50%~90% acetic acid deionized water solution into zirconium oxide by 0.1g: 1mL solid-to-liquid ratio, shaking table vibrates 1~4 hour, be centrifugally separating to obtain desorption liquid, membrane filtration, filtrate be freeze-dried to get.The available phenolic acid of the method for the present invention and all higher higher degree leaf of bamboo polyphenol of flavones content, and its yield is also higher.This method is easy to operate, environmentally protective, low to production equipment requirement, and product cost is low, is adapted for large-scale production.
Description
Technical field
The present invention relates to leaf of bamboo extracts, and in particular to a method of leaf of bamboo polyphenol is prepared from the leaf of bamboo.
Background technique
Bamboo is widely distributed in China, and leaf not only has ornamental value, is that Chinese medicine is common there are also important medical value
Heat-clearing and detoxifying herb simply.Polyphenol compound leaf of bamboo polyphenol is active constituent important in the leaf of bamboo, mainly by phenolic acid class
Close the composition such as object and flavone compound.Phenolic acid in the leaf of bamboo common are chlorogenic acid, caffeic acid, p-Coumaric Acid and ferulic acid
Deng not only having and remove interior free yl, eliminate fatigue, adjust immunity of organisms, anti-aging, protection liver, adjust blood lipid, is anti-
Angiocardiopathy and other effects also has inhibiting bacteria and diminishing inflammation, promotes epidermal cell proliferation, repair skin injury, inhibit B16 cell
With the activity of ecchymose removing whitening.Flavones in the leaf of bamboo mainly includes Lutonaretin and orientoside etc., is not only had anti-oxidant, antiviral
With it is antitumor and other effects, also have the function for the treatment of intestines problem and prophylactic treatment diabetes.Therefore, in the leaf of bamboo phenolic acid and
Flavones is carried out while being separated, and both preparations all very high leaf of bamboo polyphenol of content has in the fields such as food additives and health care product
Significance.
In the separation method of leaf of bamboo polyphenol, most commonly resin adsorption method at present, but due to phenolic acid class in the leaf of bamboo
The polarity spectrum for closing object and flavone compound is larger, and the leaf of bamboo polyphenol isolated for a certain absorption resin, there are flavones
Content is very high and problem that phenolic acid is very low, or opposite.Method there is no from bamboo extractive while phenol can be isolated at present
Acid and all very high leaf of bamboo polyphenol of flavones content, limit the use of the product.Therefore, be badly in need of develop one kind can be from the leaf of bamboo
The method for preparing leaf of bamboo polyphenol of separation phenolic acid and flavones is extracted simultaneously.
Summary of the invention
For the deficiencies in the prior art, technical problem to be solved by the invention is to provide one kind to make from the leaf of bamboo
The method of standby leaf of bamboo polyphenol, not only its yield is higher for the leaf of bamboo polyphenol of this method preparation, and leaf of bamboo phenolic acid therein and the leaf of bamboo
Flavones content is higher, and this method also has the advantages that easy to operate, environmentally friendly.
The scheme that the present invention solves above-mentioned technical problem is:
A method of preparing leaf of bamboo polyphenol from the leaf of bamboo, this method comprises the steps of:
(1) leaf of bamboo powder is taken, it is molten that the ethyl alcohol that volumetric concentration is 30%~70% is added by the solid-to-liquid ratio of 1g: 10~20mL
Liquid, ultrasonic extraction, extracting solution obtain crude extract through membrane filtration;
(2) zirconium oxide, shaking table oscillation 1 are added into crude extract in the ratio that 0.2~0.5g zirconium oxide is added in 1mL crude extract
~4 hours, it is centrifugated out liquid, collects zirconium oxide;
Wherein, the zirconium oxide is the mixture of monoclinic system and cubic phase, ir data (KBr) are as follows:
500-850,1200-1460,1460-1680 (cm-1);
Above-mentioned zirconium oxide is made by following methods:
A) by ZrOCl2·8H2O is dissolved in deionization H2O is configured to ZrOCl2Concentration be 0.2~0.6mol/L solution,
The ammonium hydroxide of 28%wt is slowly added under stirring, until pH is 10;Obtained white suspension continues to stir, until being precipitated completely white
Color precipitating;
B) white depositions are washed with deionized to pH=7, is put into baking oven and is dried at 110 DEG C, then be placed in Muffle
300~600 DEG C of calcining 2 hours zirconium oxides to get white in furnace;
(3) by after collected zirconium oxide ethanol washing, by 0.1g: 1mL solid-to-liquid ratio into the zirconium oxide after washing
The aqueous acetic acid that volume ratio is 1~9 ︰ 1 of Cu Suan ︰ deionized water=1 ︰ is added, shaking table is vibrated 1~4 hour, is centrifugally separating to obtain
Desorption liquid, membrane filtration, filtrate are freeze-dried to get leaf of bamboo polyphenol.
It is of the present invention from the method for preparing leaf of bamboo polyphenol in the leaf of bamboo, the power and volume of material of the ultrasonic extraction
Than being 2.5~5W: 1mL, the time of ultrasonic extraction is 40~80 minutes.
It is of the present invention from the method for preparing leaf of bamboo polyphenol in the leaf of bamboo, shaking table described in step (2) and (3) concussion
Operating temperature is 37 DEG C, and revolving speed is 150rpm.
The method of the present invention that leaf of bamboo polyphenol is prepared from the leaf of bamboo is raw material using the leaf of bamboo, ultrasonic in ethanol solution
After extraction, selective oxidation zirconium is adsorbent, and by absorption, washing, desorption and freeze-drying, it is more greater than 80% leaf of bamboo can to prepare purity
Phenol, wherein phenolic acid compound content is greater than 45%, and flavonoid content is greater than 35%, and yield also reaches 0.80%
More than.
Method of the present invention does not use other any organic reagents in addition to ethyl alcohol and acetic acid, is a kind of environment friend
The separation method of good type.The method of the present invention is easy to operate, low without putting into expensive production facility, product cost, is suitable for industry
Metaplasia produces.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of the zirconium oxide prepared in the embodiment of the present invention 1.
Fig. 2 is the X-ray crystallogram of the zirconium oxide prepared in the embodiment of the present invention 1.
Fig. 3 is the HPLC map and standard items HPLC map comparison diagram of leaf of bamboo polyphenol obtained in the embodiment of the present invention 1.
Specific embodiment
Embodiment 1
One, the preparation of zirconium oxide
1, solid ZrOCl2·8H2O (12.89g, 0.04mol) is dissolved in (ZrOCl after the deionized water of 94mL2Concentration is
0.4mol/L), the ammonium hydroxide of 28%wt is added dropwise, until pH=10, obtained white suspension continues to be stirred at room temperature 1 small
When;
2, the white precipitate that 3500rpm is centrifuged is washed with deionized to pH=7, in an oven 110 DEG C of heating
12h calcines 2 hours in Muffle furnace to get white oxide zirconium for 400 DEG C.
Two, the characterization of zirconium oxide
1, step 1 preparation zirconium oxide using infrared spectrometer detection after, infrared spectroscopy (KBr) as shown in Fig. 1,
Its ir data (KBr) are as follows: 500-850,1200-1460,1460-1680 (cm-1);
2, after the zirconium oxide of step 1 preparation is using the detection of X crystal diffraction instrument, XRD spectrum is as shown in Fig. 2: this method
The zirconium oxide of preparation is the mixture of monoclinic system and cubic phase.
Three, the preparation of leaf of bamboo polyphenol
1, the Moso Bamboo Leaves powder 1g of 40 meshes was taken, the ethanol solution 10mL that volumetric concentration is 70% is added, in 50W/
Ultrasonic extraction 60 minutes under 45kHz;Extracting solution obtains crude extract after 0.45 μm of membrane filtration.
2, the zirconium oxide that 0.4g step 1 obtains is added by 1mL crude extract, under conditions of 37 DEG C/150rpm, in concussion
Oscillation absorption 1 hour on shaking table;4000rpm is centrifuged 1 minute, collects the zirconium oxide isolated.
3, by the zirconium oxide of collection with 4mL ethanol washing 2 times, the then oxidation by 0.1g: 1mL solid-to-liquid ratio toward after washing
The acetic acid deionized water solution that volumetric concentration is 70% is added in zirconium, under the conditions of 37 DEG C/150rpm, is vibrated on concussion shaking table
Desorption 1 hour;After 4000rpm is centrifuged 1 minute, obtained 0.22 μm of membrane filtration of desorption liquid, after filtrate is freeze-dried
To the leaf of bamboo polyphenol 13.5mg of light yellow powder.
Four, the purity detecting of leaf of bamboo polyphenol:
The leaf of bamboo polyphenol that step 3 obtains is dissolved in the aqueous acetic acid of 0.8% (volume fraction), uses efficient liquid phase
Chromatograph analyzes sample purity.Chromatographic condition is as follows: chromatographic column is Agilent HC-C18 (250 × 4.6mm, 5 μm);Stream
Dynamic phase A is acetonitrile, and Mobile phase B is the aqueous acetic acid of 0.8% (volume fraction);0~10 minute, mobile phase A was increased by 5% gradient
It is added to 15%;10~20 minutes, mobile phase A holding 15% was constant, and 20~25 minutes, mobile phase A was increased to by 15% gradient
20%;25~35 minutes, mobile phase A holding 20% was constant;35~40 minutes, mobile phase A increased to 40% by 20% gradient;40
~45 minutes, mobile phase A holding 40% was constant;45~50 minutes, mobile phase was reduced to 5% by 40% gradient;50~55 minutes,
Mobile phase A holding 5% is constant;Detection wavelength is 330nm, and flow velocity is 1mL/ minutes.
Testing result (the standard items HPLC map with neochlorogenic acid, chlorogenic acid, Cryptochlorogenic acid, Lutonaretin and orientoside
Comparative diagram) as shown in Fig. 3, show leaf of bamboo polyphenol in buff powder made from the present embodiment content be 87%, wherein
Polyphenol Acids kind compound content is 48%, Flavone content 39%, and the yield of leaf of bamboo polyphenol is 1.17%.
Wherein, the yield (%) of the leaf of bamboo polyphenol=(hundred of total polyphenols in leaf of bamboo polyphenol freeze-dried powder quality × freeze-dried powder
Divide content)/leaf of bamboo dry weight × 100 (1)
The leaf of bamboo polyphenol includes leaf of bamboo phenolic acid and bamboo-leaves flavones, and content calculates as follows respectively:
Leaf of bamboo polyphenol content (%)=leaf of bamboo polyphenol chromatographic peak area/all chromatographic peak area × 100 (2)
Leaf of bamboo phenolic content (%)=leaf of bamboo phenolic acid chromatographic peak area/all chromatographic peak area × 100 (3)
The leaf of bamboo phenolic acid includes 3 kinds of neochlorogenic acid, chlorogenic acid and Cryptochlorogenic acid main phenolic acid compounds.
Bamboo-leaves flavones content (%)=bamboo-leaves flavones chromatographic peak area/all chromatographic peak area × 100 (4)
The bamboo-leaves flavones include 2 kinds of Main Flavonoids class compounds of Lutonaretin and orientoside.
Embodiment 2
One, the preparation of zirconium oxide:
In this example zirconium oxide preparation method difference from example 1 is that: ZrOCl2Concentration be 0.6mol/
L, the calcination temperature of zirconium oxide are 500 degree, remaining step is same as Example 1.
Two, the preparation of leaf of bamboo polyphenol:
1, the Lophatherum Herb 1g of 40 meshes was taken, the ethanol solution 20mL that volumetric concentration is 50% is added, in 50W/
Ultrasonic extraction 40 minutes under 45kHz;Extracting solution obtains crude extract after 0.45 μm of membrane filtration.
2, the zirconium oxide that step 1 obtains is added into crude extract in the ratio that 0.2g zirconium oxide is added in 1mL crude extract,
Under conditions of 37 DEG C/150rpm, in oscillation absorption 2 hours on concussion shaking table;4000rpm is centrifuged 1 minute, collects the oxygen isolated
Change zirconium.
3, by the zirconium oxide of collection with 4mL ethanol washing 2 times, the then oxidation by 0.1g: 1mL solid-to-liquid ratio toward after washing
The acetic acid deionized water solution that volumetric concentration is 90% is added in zirconium, under the conditions of 37 DEG C/150rpm, is vibrated on concussion shaking table
Desorption 2 hours;After 4000rpm is centrifuged 1 minute, obtained 0.22 μm of membrane filtration of desorption liquid, after filtrate is freeze-dried
To light yellow powder leaf of bamboo polyphenol 10.2mg.
Content detection is carried out using the same method of embodiment 1, the results show that the leaf of bamboo is more in obtained buff powder
The content of phenol is 83%, and wherein polyphenol compound content is 47%, and the yield of Flavone content 36%, leaf of bamboo polyphenol is
0.85%.
Embodiment 3
One, the preparation of zirconium oxide:
In this example zirconium oxide preparation method difference from example 1 is that: ZrOCl2Concentration be 0.8mol/
L, the calcination temperature of zirconium oxide are 300 degree, remaining step is same as Example 1.
Two, the preparation of leaf of bamboo polyphenol:
1, the Lophatherum Herb 1g of 40 meshes was taken, the ethanol solution 15mL that volumetric concentration is 70% is added, in 50W/
Ultrasonic extraction 50 minutes under 45kHz;Extracting solution obtains crude extract after 0.45 μm of membrane filtration.
2, the zirconium oxide that step 1 obtains is added into crude extract in the ratio that 0.3g zirconium oxide is added in 1mL crude extract,
Under conditions of 37 DEG C/150rpm, in oscillation absorption 4 hours on concussion shaking table;4000rpm is centrifuged 1 minute, collects the oxygen isolated
Change zirconium.
3, by the zirconium oxide of collection with 4mL ethanol washing 2 times, the then oxidation by 0.1g: 1mL solid-to-liquid ratio toward after washing
The acetic acid deionized water solution that volumetric concentration is 50% is added in zirconium, under the conditions of 37 DEG C/150rpm, is vibrated on concussion shaking table
Desorption 4 hours;After 4000rpm is centrifuged 1 minute, obtained 0.22 μm of membrane filtration of desorption liquid, after filtrate is freeze-dried
To light yellow powder leaf of bamboo polyphenol 11.3mg.
Content detection is carried out using the same method of embodiment 1, the results show that the leaf of bamboo is more in obtained buff powder
The content of phenol is 86%, and wherein polyphenol compound content is 46%, and the yield of Flavone content 40%, leaf of bamboo polyphenol is
0.97%.
Embodiment 4
One, the preparation of zirconium oxide:
In this example zirconium oxide preparation method difference from example 1 is that: ZrOCl2Concentration be 0.6mol/
L, the calcination temperature of zirconium oxide are 600 degree, remaining step is same as Example 1.
Two, the preparation of leaf of bamboo polyphenol:
1, the Moso Bamboo Leaves powder 1g of 40 meshes was taken, the ethanol solution 10mL that volumetric concentration is 30% is added, in 50W/
Ultrasonic extraction 40 minutes under 45kHz;Extracting solution obtains crude extract after 0.45 μm of membrane filtration.
2, the zirconium oxide that step 1 obtains is added into crude extract in the ratio that 0.3g zirconium oxide is added in 1mL crude extract,
Under conditions of 37 DEG C/150rpm, in oscillation absorption 1 hour on concussion shaking table;4000rpm is centrifuged 1 minute, collects the oxygen isolated
Change zirconium.
3, by the zirconium oxide of collection with 4mL ethanol washing 2 times, the then oxidation by 0.1g: 1mL solid-to-liquid ratio toward after washing
The acetic acid deionized water solution that volumetric concentration is 70% is added in zirconium, under the conditions of 37 DEG C/150rpm, is vibrated on concussion shaking table
Desorption 1 hour;After 4000rpm is centrifuged 1 minute, obtained 0.22 μm of membrane filtration of desorption liquid, after filtrate is freeze-dried
To light yellow powder leaf of bamboo polyphenol 9.86mg.
Content detection is carried out using the same method of embodiment 1, the results show that the leaf of bamboo is more in obtained buff powder
The content of phenol is 83%, and wherein polyphenol compound content is 46%, and the yield of Flavone content 37%, leaf of bamboo polyphenol is
0.82%.
Embodiment 5
One, the preparation of zirconium oxide:
The preparation method of zirconium oxide is same as Example 1 in this example.
Two, the preparation of leaf of bamboo polyphenol:
1, the Moso Bamboo Leaves powder 1g of 40 meshes was taken, the ethanol solution 10mL that volumetric concentration is 70% is added, in 50W/
Ultrasonic extraction 60 minutes under 45kHz;Extracting solution obtains crude extract after 0.45 μm of membrane filtration.
2, the zirconium oxide that step 1 obtains is added into crude extract in the ratio that 0.4g zirconium oxide is added in 1mL crude extract,
Under conditions of 37 DEG C/150rpm, in oscillation absorption 1 hour on concussion shaking table;4000rpm is centrifuged 1 minute, collects the oxygen isolated
Change zirconium.
3, by the zirconium oxide of collection with 4mL ethanol washing 2 times, the then oxidation by 0.1g: 1mL solid-to-liquid ratio toward after washing
The acetic acid deionized water solution that volumetric concentration is 90% is added in zirconium, under the conditions of 37 DEG C/150rpm, is vibrated on concussion shaking table
Desorption 1 hour;After 4000rpm is centrifuged 1 minute, obtained 0.22 μm of membrane filtration of desorption liquid, after filtrate is freeze-dried
To light yellow powder leaf of bamboo polyphenol 12.1mg.
Content detection is carried out using the same method of embodiment 1, the results show that the leaf of bamboo is more in obtained buff powder
The content of phenol is 85%, and wherein polyphenol compound content is 48%, and the yield of Flavone content 37%, leaf of bamboo polyphenol is
1.03%.
Embodiment 6
One, the preparation of zirconium oxide:
The preparation method with embodiment 1 of zirconium oxide is identical in this example.
Two, the preparation of leaf of bamboo polyphenol:
1, the Moso Bamboo Leaves powder 1g of 40 meshes was taken, the ethanol solution 20mL that volumetric concentration is 70% is added, in 50W/
Ultrasonic extraction 80 minutes under 45kHz;Extracting solution obtains crude extract after 0.45 μm of membrane filtration.
2, the zirconium oxide that step 1 obtains is added into crude extract in the ratio that 0.5g zirconium oxide is added in 1mL crude extract,
Under conditions of 37 DEG C/150rpm, in oscillation absorption 1 hour on concussion shaking table;4000rpm is centrifuged 1 minute, collects the oxygen isolated
Change zirconium.
3, by the zirconium oxide of collection with 4mL ethanol washing 2 times, the then oxidation by 0.1g: 1mL solid-to-liquid ratio toward after washing
The acetic acid deionized water solution that volumetric concentration is 50% is added in zirconium, under the conditions of 37 DEG C/150rpm, is vibrated on concussion shaking table
Desorption 1 hour;After 4000rpm is centrifuged 1 minute, obtained 0.22 μm of membrane filtration of desorption liquid, after filtrate is freeze-dried
To light yellow powder leaf of bamboo polyphenol 10.5mg.
Content detection is carried out using the same method of embodiment 1, the results show that the leaf of bamboo is more in obtained buff powder
The content of phenol is 82%, and wherein polyphenol compound content is 46%, and the yield of Flavone content 36%, leaf of bamboo polyphenol is
0.86%.
Claims (3)
1. a kind of method for preparing leaf of bamboo polyphenol from the leaf of bamboo, this method comprise the steps of:
(1) leaf of bamboo powder is taken, the ethanol solution that volumetric concentration is 30%~70%, ultrasound is added by the solid-to-liquid ratio of 1g: 10~20mL
It extracts, extracting solution obtains crude extract through membrane filtration;
(2) zirconium oxide, shaking table oscillation 1~4 are added into crude extract in the ratio that 0.2~0.5g zirconium oxide is added in 1mL crude extract
Hour, it is centrifugated out liquid, collects zirconium oxide;
Wherein, the zirconium oxide is the mixture of monoclinic system and cubic phase, ir data (KBr) are as follows: 500-
850,1200-1460,1460-1680(cm-1);
Above-mentioned zirconium oxide is made by following methods:
A) by ZrOCl2·8H2O is dissolved in deionization H2O is configured to ZrOCl2Concentration be 0.2~0.6mol/L solution, stirring
Under be slowly added to the ammonium hydroxide of 28%wt, until pH is 10;Obtained white suspension continues to stir, until it is heavy that white is precipitated completely
It forms sediment;
B) white depositions are washed with deionized to pH=7, is put into baking oven and is dried at 110 DEG C, then be placed in Muffle furnace
300~600 DEG C of calcining 2 hours zirconium oxides to get white;
(3) it by after collected zirconium oxide ethanol washing, is added by 0.1g: 1mL solid-to-liquid ratio into the zirconium oxide after washing
Volume ratio is the aqueous acetic acid of 1~9 ︰ 1 of Cu Suan ︰ deionized water=1 ︰, and shaking table vibrates 1~4 hour, is centrifugally separating to obtain desorption
Liquid, membrane filtration, filtrate are freeze-dried to get leaf of bamboo polyphenol.
2. the method for leaf of bamboo polyphenol is prepared from the leaf of bamboo according to claim 1, it is characterised in that: the ultrasonic extraction
Power and volume of material ratio are 2.5~5W: 1mL, and the time of ultrasonic extraction is 40~80 minutes.
3. the method for leaf of bamboo polyphenol is prepared from the leaf of bamboo according to claim 1, it is characterised in that: institute in step (2) and (3)
The operating temperature for the shaking table concussion stated is 37 DEG C, and revolving speed is 150rpm.
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CN101391060A (en) * | 2008-11-05 | 2009-03-25 | 中国林业科学研究院林产化学工业研究所 | Preparation method of bamboo leaf flavone |
CN101531904A (en) * | 2009-05-05 | 2009-09-16 | 国际竹藤网络中心 | Bamboo leaves extract, preparing method and purpose thereof |
CN102861256A (en) * | 2012-09-27 | 2013-01-09 | 武汉神农天香生物科技有限公司 | Method for preparing flavone from bamboo leaves |
CN104357952A (en) * | 2014-11-21 | 2015-02-18 | 浙江和也健康科技有限公司 | Bamboo leaf flavonoid mint core-sheath compound fiber |
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CN101391060A (en) * | 2008-11-05 | 2009-03-25 | 中国林业科学研究院林产化学工业研究所 | Preparation method of bamboo leaf flavone |
CN101531904A (en) * | 2009-05-05 | 2009-09-16 | 国际竹藤网络中心 | Bamboo leaves extract, preparing method and purpose thereof |
CN102861256A (en) * | 2012-09-27 | 2013-01-09 | 武汉神农天香生物科技有限公司 | Method for preparing flavone from bamboo leaves |
CN104357952A (en) * | 2014-11-21 | 2015-02-18 | 浙江和也健康科技有限公司 | Bamboo leaf flavonoid mint core-sheath compound fiber |
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