CN107118102A - A kind of method that leaf of bamboo polyphenol is prepared from the leaf of bamboo - Google Patents

A kind of method that leaf of bamboo polyphenol is prepared from the leaf of bamboo Download PDF

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CN107118102A
CN107118102A CN201710246445.1A CN201710246445A CN107118102A CN 107118102 A CN107118102 A CN 107118102A CN 201710246445 A CN201710246445 A CN 201710246445A CN 107118102 A CN107118102 A CN 107118102A
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leaf
bamboo
zirconium oxide
polyphenol
shaking table
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CN107118102B (en
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马意龙
商亚芳
刘凤茹
朱丹晔
王彩虹
刘帅
潘少山
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Hefei University of Technology
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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
    • 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
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The present invention relates to leaf of bamboo extract, and in particular to the method that leaf of bamboo polyphenol is prepared from the leaf of bamboo.This method is comprised the steps of：(1) leaf of bamboo powder is taken to add ethanol solution by 1g: 10~20mL solid-to-liquid ratio, ultrasonic extraction, membrane filtration obtains crude extract；(2) ratio for adding 0.2~0.5g zirconium oxides in 1mL crude extracts adds zirconium oxide into crude extract, and shaking table vibrates 1~4 hour, centrifuges out zirconium oxide and washed with ethanol；(3) by 0.1g: 1mL solid-to-liquid ratio toward 50%~90% acetic acid deionized water solution of addition in zirconium oxide, shaking table is vibrated 1~4 hour, is centrifugally separating to obtain desorption liquid, and membrane filtration, filtrate freeze-drying is produced.The inventive method can obtain phenolic acid and flavones content all higher higher degree leaf of bamboo polyphenol, and its yield is also higher.This method is easy to operate, environmental protection, to production equipment require it is low, product cost is low, is adapted for large-scale production.

Description

A kind of method that leaf of bamboo polyphenol is prepared from the leaf of bamboo
Technical field
The present invention relates to leaf of bamboo extract, and in particular to a kind of method that leaf of bamboo polyphenol is prepared from the leaf of bamboo.
Background technology
Bamboo is widely distributed in China, and its leaf not only has ornamental value, and also important medical value is that the traditional Chinese medical science is commonly used Heat-clearing and detoxifying herb simply.Polyphenol compound leaf of bamboo polyphenol is important active component in the leaf of bamboo, mainly by phenolic acid class Compound and flavone compound etc. are constituted.Phenolic acid in the leaf of bamboo common are chlorogenic acid, caffeic acid, p-Coumaric Acid and forulic acid Deng, not only with removing interior free yl, it is dispelling fatigue, regulation immunity of organisms, anti-aging, protection liver, regulation blood fat, anti- The effects such as angiocardiopathy, also with inhibiting bacteria and diminishing inflammation, promote epidermal cell proliferation, reparation skin injury, suppression B16 cell With the activity of ecchymose removing whitening.Flavones in the leaf of bamboo mainly includes Lutonaretin and orientoside etc., not only with anti-oxidant, antiviral And it is antitumor the effects such as, also with treatment intestines problem and prophylactic treatment diabetes effect.Therefore, to the phenolic acid in the leaf of bamboo and Flavones separate simultaneously, both prepares contents all very high leaf of bamboo polyphenol, has in the field such as food additives and health products Significance.
In the separation method of leaf of bamboo polyphenol, most commonly resin adsorption method, but be due to phenolic acid class in the leaf of bamboo at present The polarity spectrum of compound and flavone compound is larger, for the isolated leaf of bamboo polyphenol of a certain polymeric adsorbent, there is flavones Content is very high and the problem of very low phenolic acid, or conversely.It there is no method can be from bamboo extractive while isolating phenol at present Acid and flavones content all very high leaf of bamboo polyphenol, limit the use of the product.Therefore, being badly in need of development 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.
The content of the invention
For the deficiencies in the prior art, the technical problems to be solved by the invention are to provide one kind and made from the leaf of bamboo The method of standby leaf of bamboo polyphenol, not only its yield is higher for leaf of bamboo polyphenol prepared by this method, 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 present invention solve above-mentioned technical problem scheme be：
A kind of method that leaf of bamboo polyphenol is prepared from the leaf of bamboo, this method is comprised the steps of：
(1) leaf of bamboo powder is taken, it is molten for 30%~70% ethanol to add volumetric concentration by 1g: 10~20mL solid-to-liquid ratio Liquid, ultrasonic extraction, extract solution obtains crude extract through membrane filtration；
(2) ratios of 0.2~0.5g zirconium oxides is added in 1mL crude extracts toward adding zirconium oxide, shaking table vibration 1 in crude extract ~4 hours, liquid is centrifuged out, zirconium oxide is collected；
Wherein, described zirconium oxide is the mixture of monoclinic system and Emission in Cubic, and its ir data (KBr) is： 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, 28%wt ammoniacal liquor is slowly added under stirring, until pH is 10；Obtained white suspension continues to stir, until separating out completely white Color is precipitated；
B) white depositions are washed with deionized to pH=7, is put into baking oven at 110 DEG C and dries, then be placed in Muffle Calcined 2 hours for 300~600 DEG C in stove, produce the zirconium oxide of white；
(3) after collected zirconium oxide is washed with ethanol, by zirconium oxide of 0.1g: the 1mL solid-to-liquid ratio toward after washing Addition volume ratio is Cu Suan ︰ deionized waters=︰ 1 of 1 ︰ 1~9 aqueous acetic acid, and shaking table vibrates 1~4 hour, is centrifugally separating to obtain Desorption liquid, membrane filtration, filtrate freeze-drying produces leaf of bamboo polyphenol.
In the method for the present invention that leaf of bamboo polyphenol is prepared from the leaf of bamboo, the power and volume of material of described ultrasonic extraction It it is 40~80 minutes than the time for 2.5~5W: 1mL, ultrasonic extraction.
In the method for the present invention that leaf of bamboo polyphenol is prepared from the leaf of bamboo, what the shaking table described in step (2) and (3) shook Operating temperature is 37 DEG C, and rotating 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, by absorption, washing, is desorbed and lyophilized, can prepare the leaf of bamboo of the purity more than 80% many Phenol, wherein phenolic acid compound content are more than 45%, and flavonoid content is more than 35%, and yield also reaches 0.80% More than.
Method of the present invention is in addition to ethanol and acetic acid, not using other any organic reagents, is a kind of environment friend The separation method of good type.The inventive method production facility simple to operate, expensive without input, product cost are low, suitable for industry Metaplasia is produced.
Brief description of the drawings
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 collection of illustrative plates and standard items HPLC collection of illustrative plates comparison diagrams of obtained leaf of bamboo polyphenol in the embodiment of the present invention 1.
Embodiment
Embodiment 1
First, the preparation of zirconium oxide
1st, solid ZrOCl2·8H2O (12.89g, 0.04mol) is dissolved in after 94mL deionized water (ZrOCl2Concentration is 0.4mol/L), 28%wt ammoniacal liquor is added dropwise, until pH=10, obtained white suspension continues to be stirred at room temperature 1 small When；
2nd, the white precipitate that 3500rpm centrifugations are obtained is washed with deionized to pH=7, in an oven 110 DEG C of heating 12h, calcines 2 hours for 400 DEG C in Muffle furnace, produces white oxide zirconium.
2nd, the sign of zirconium oxide
1st, step one prepare zirconium oxide using infrared spectrometer detection after, its infrared spectrum (KBr) as shown in Figure 1, Its ir data (KBr) is：500-850,1200-1460,1460-1680 (cm-1)；
2nd, after zirconium oxide prepared by step one is using the detection of X crystal diffractions instrument, its XRD spectrum is as shown in Figure 2：This method The zirconium oxide of preparation is the mixture of monoclinic system and Emission in Cubic.
3rd, the preparation of leaf of bamboo polyphenol
1st, the Moso Bamboo Leaves powder 1g of 40 mesh sieves was taken, the ethanol solution 10mL that volumetric concentration is 70% is added, in 50W/ Ultrasonic extraction 60 minutes under 45kHz；Extract solution obtains crude extract after 0.45 μm of membrane filtration.
2nd, the zirconium oxide that 0.4g steps one are obtained is added by 1mL crude extracts, under conditions of 37 DEG C/150rpm, in concussion Vibration absorption 1 hour on shaking table；4000rpm is centrifuged 1 minute, collects the zirconium oxide isolated.
3rd, the zirconium oxide of collection is washed 2 times with 4mL ethanol, 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 desorption liquid is obtained with 0.22 μm of membrane filtration after filtrate is freeze-dried To the leaf of bamboo polyphenol 13.5mg of light yellow powder.
4th, the purity detecting of leaf of bamboo polyphenol：
The leaf of bamboo polyphenol that step 3 is obtained is dissolved in the aqueous acetic acid of 0.8% (volume fraction), uses efficient liquid phase Chromatograph is analyzed 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 collection of illustrative plates with neochlorogenic acid, chlorogenic acid, Cryptochlorogenic acid, Lutonaretin and orientoside Compares figure) as shown in Figure 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%, and Flavone content is 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 its content is calculated 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 neochlorogenic acid, chlorogenic acid and the main phenolic acid compound of 3 kinds of Cryptochlorogenic acid.
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
First, the preparation of zirconium oxide：
The difference of the preparation method of zirconium oxide and embodiment 1 is in this example：ZrOCl2Concentration be 0.6mol/ L, the calcining heat of zirconium oxide is 500 degree, and remaining step is same as Example 1.
2nd, the preparation of leaf of bamboo polyphenol：
1st, the Lophatherum Herb 1g of 40 mesh sieves was taken, the ethanol solution 20mL that volumetric concentration is 50% is added, in 50W/ Ultrasonic extraction 40 minutes under 45kHz；Extract solution obtains crude extract after 0.45 μm of membrane filtration.
2nd, the ratios of 0.2g zirconium oxides is added in 1mL crude extracts toward adding the zirconium oxide that step one is obtained in crude extract, Under conditions of 37 DEG C/150rpm, in vibration absorption 2 hours on concussion shaking table；4000rpm is centrifuged 1 minute, collects the oxygen isolated Change zirconium.
3rd, the zirconium oxide of collection is washed 2 times with 4mL ethanol, 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 desorption liquid is obtained with 0.22 μm of membrane filtration 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, as a result shown, the leaf of bamboo is more in resulting buff powder The content of phenol is 83%, and wherein polyphenol compound content is 47%, and Flavone content is 36%, and the yield of leaf of bamboo polyphenol is 0.85%.
Embodiment 3
First, the preparation of zirconium oxide：
The difference of the preparation method of zirconium oxide and embodiment 1 is in this example：ZrOCl2Concentration be 0.8mol/ L, the calcining heat of zirconium oxide is 300 degree, and remaining step is same as Example 1.
2nd, the preparation of leaf of bamboo polyphenol：
1st, the Lophatherum Herb 1g of 40 mesh sieves was taken, the ethanol solution 15mL that volumetric concentration is 70% is added, in 50W/ Ultrasonic extraction 50 minutes under 45kHz；Extract solution obtains crude extract after 0.45 μm of membrane filtration.
2nd, the ratios of 0.3g zirconium oxides is added in 1mL crude extracts toward adding the zirconium oxide that step one is obtained in crude extract, Under conditions of 37 DEG C/150rpm, in vibration absorption 4 hours on concussion shaking table；4000rpm is centrifuged 1 minute, collects the oxygen isolated Change zirconium.
3rd, the zirconium oxide of collection is washed 2 times with 4mL ethanol, 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 desorption liquid is obtained with 0.22 μm of membrane filtration 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, as a result shown, the leaf of bamboo is more in resulting buff powder The content of phenol is 86%, and wherein polyphenol compound content is 46%, and Flavone content is 40%, and the yield of leaf of bamboo polyphenol is 0.97%.
Embodiment 4
First, the preparation of zirconium oxide：
The difference of the preparation method of zirconium oxide and embodiment 1 is in this example：ZrOCl2Concentration be 0.6mol/ L, the calcining heat of zirconium oxide is 600 degree, and remaining step is same as Example 1.
2nd, the preparation of leaf of bamboo polyphenol：
1st, the Moso Bamboo Leaves powder 1g of 40 mesh sieves was taken, the ethanol solution 10mL that volumetric concentration is 30% is added, in 50W/ Ultrasonic extraction 40 minutes under 45kHz；Extract solution obtains crude extract after 0.45 μm of membrane filtration.
2nd, the ratios of 0.3g zirconium oxides is added in 1mL crude extracts toward adding the zirconium oxide that step one is obtained in crude extract, Under conditions of 37 DEG C/150rpm, in vibration absorption 1 hour on concussion shaking table；4000rpm is centrifuged 1 minute, collects the oxygen isolated Change zirconium.
3rd, the zirconium oxide of collection is washed 2 times with 4mL ethanol, 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 desorption liquid is obtained with 0.22 μm of membrane filtration 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, as a result shown, the leaf of bamboo is more in resulting buff powder The content of phenol is 83%, and wherein polyphenol compound content is 46%, and Flavone content is 37%, and the yield of leaf of bamboo polyphenol is 0.82%.
Embodiment 5
First, the preparation of zirconium oxide：
The preparation method of zirconium oxide is same as Example 1 in this example.
2nd, the preparation of leaf of bamboo polyphenol：
1st, the Moso Bamboo Leaves powder 1g of 40 mesh sieves was taken, the ethanol solution 10mL that volumetric concentration is 70% is added, in 50W/ Ultrasonic extraction 60 minutes under 45kHz；Extract solution obtains crude extract after 0.45 μm of membrane filtration.
2nd, the ratios of 0.4g zirconium oxides is added in 1mL crude extracts toward adding the zirconium oxide that step one is obtained in crude extract, Under conditions of 37 DEG C/150rpm, in vibration absorption 1 hour on concussion shaking table；4000rpm is centrifuged 1 minute, collects the oxygen isolated Change zirconium.
3rd, the zirconium oxide of collection is washed 2 times with 4mL ethanol, 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 desorption liquid is obtained with 0.22 μm of membrane filtration 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, as a result shown, the leaf of bamboo is more in resulting buff powder The content of phenol is 85%, and wherein polyphenol compound content is 48%, and Flavone content is 37%, and the yield of leaf of bamboo polyphenol is 1.03%.
Embodiment 6
First, the preparation of zirconium oxide：
The preparation method of zirconium oxide is identical with embodiment 1 in this example.
2nd, the preparation of leaf of bamboo polyphenol：
1st, the Moso Bamboo Leaves powder 1g of 40 mesh sieves was taken, the ethanol solution 20mL that volumetric concentration is 70% is added, in 50W/ Ultrasonic extraction 80 minutes under 45kHz；Extract solution obtains crude extract after 0.45 μm of membrane filtration.
2nd, the ratios of 0.5g zirconium oxides is added in 1mL crude extracts toward adding the zirconium oxide that step one is obtained in crude extract, Under conditions of 37 DEG C/150rpm, in vibration absorption 1 hour on concussion shaking table；4000rpm is centrifuged 1 minute, collects the oxygen isolated Change zirconium.
3rd, the zirconium oxide of collection is washed 2 times with 4mL ethanol, 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 desorption liquid is obtained with 0.22 μm of membrane filtration 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, as a result shown, the leaf of bamboo is more in resulting buff powder The content of phenol is 82%, and wherein polyphenol compound content is 46%, and Flavone content is 36%, and the yield of leaf of bamboo polyphenol is 0.86%.

Claims (3)

1. a kind of method that leaf of bamboo polyphenol is prepared from the leaf of bamboo, this method is comprised the steps of：
(1) leaf of bamboo end is taken, the ethanol solution that volumetric concentration is 30%~70%, ultrasound are added by 1g: 10~20mL solid-to-liquid ratio Extract, extract solution obtains crude extract through membrane filtration；
(2) ratios of 0.2~0.5g zirconium oxides is added in 1mL crude extracts toward adding zirconium oxide, shaking table vibration 1~4 in crude extract Hour, liquid is centrifuged out, zirconium oxide is collected；
Wherein, described zirconium oxide is the mixture of monoclinic system and Emission in Cubic, and its ir data (KBr) is：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 28%wt ammoniacal liquor, until pH is 10；Obtained white suspension continues to stir, until it is heavy to separate out white completely Form sediment；
B) white depositions are washed with deionized to pH=7, is put into baking oven at 110 DEG C and dries, then be placed in Muffle furnace 300~600 DEG C are calcined 2 hours, produce the zirconium oxide of white；
(3) after collected zirconium oxide is washed with ethanol, by addition in zirconium oxide of 0.1g: the 1mL solid-to-liquid ratio toward after washing Volume ratio is Cu Suan ︰ deionized waters=︰ 1 of 1 ︰ 1~9 aqueous acetic acid, and shaking table vibrates 1~4 hour, is centrifugally separating to obtain desorption Liquid, membrane filtration, filtrate freeze-drying produces 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：Described ultrasonic extraction Power is 2.5~5W: 1mL with volume of material ratio, 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 rotating speed is 150rpm.
CN201710246445.1A 2017-04-15 2017-04-15 A method of preparing leaf of bamboo polyphenol from the leaf of bamboo Active CN107118102B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111471076A (en) * 2020-05-14 2020-07-31 合肥工业大学 Method for separating and preparing flavonoid compound from pueraria lobata flower

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111471076A (en) * 2020-05-14 2020-07-31 合肥工业大学 Method for separating and preparing flavonoid compound from pueraria lobata flower

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