CN108211417A - A kind of plant extract flavones extraction adminicle and preparation method and application - Google Patents

A kind of plant extract flavones extraction adminicle and preparation method and application Download PDF

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Publication number
CN108211417A
CN108211417A CN201810087701.1A CN201810087701A CN108211417A CN 108211417 A CN108211417 A CN 108211417A CN 201810087701 A CN201810087701 A CN 201810087701A CN 108211417 A CN108211417 A CN 108211417A
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extraction
adminicle
flavones
ethyl alcohol
parts
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CN108211417B (en
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张立攀
章建军
周莉
李彬
张亚勋
王永
郭青照
李博闻
付有利
李小云
冯军伟
李远远
冯俊旗
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HENAN INSTITUTE OF BUSINESS SCIENCE
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HENAN INSTITUTE OF BUSINESS SCIENCE
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0288Applications, solvents

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

A kind of plant extract flavones extraction adminicle, is made of the raw material of following parts by weight:1 part of nanometer hydroxyapatite, 1.5~2 parts of nano silicon dioxide, 3~5 parts of βAl2O3,3~5 parts of nano-titanium dioxide.The extracting flavonoids adminicle component of the present invention is simple, and non-toxic, safety is good, at low cost, and prepares simple;The recovery rate height of the extracting flavonoids adminicle extraction flavones of the present invention, is directly filtered after extraction, and post processing is simple and convenient, and the residue for extracting adminicle and extract passes through recyclable recycling after calcining removing residue.

Description

A kind of plant extract flavones extraction adminicle and preparation method and application
Technical field
Present invention relates particularly to a kind of plant extract flavones extraction adminiclies and preparation method and application.
Background technology
In the prior art, in the extraction process of flavones, if hot water extracts, extracting solution is perishable rotten, the reason is that using water Make solvent, easily the ingredients such as carbohydrate, protein are leached out, cause to go mouldy;If using ethyl alcohol extraction instead, though it is easily mould that water is overcome to carry The shortcomings that change, but there are the trivial operations such as subsequent filter, drying, solvent recovery;And ethyl acetate extraction method recovery rate is relatively low, and Cost is higher.Though the recovery rate of methanol extraction is high, cost is also high, and methanol is toxic, and complex process is not suitable for persimmon leaf The extraction of chromocor compound.
Invention content
The goal of the invention of the present invention is to provide a kind of plant extract flavones extraction adminicle, at the same provide preparation method and Using the another goal of the invention for being the present invention.
For achieving the above object, the technical solution taken of the present invention is:
A kind of plant extract flavones extraction adminicle, is made of the raw material of following parts by weight:1 part of nanometer hydroxyapatite, receives Rice silica 1 .5~2 part, 3~5 parts of beta-alumina, 3~5 parts of nano-titanium dioxide.
The plant extract flavones preparation method of extraction adminicle, is made by following steps:A)By nano-hydroxy Apatite is placed in 3~4 h of boiling reflux in low-carbon alcohols, adds nano silicon dioxide, and 5~6 h of boiling reflux is concentrated after cooling Remove low-carbon alcohols;B)Add in beta-alumina, nano-titanium dioxide grinding, prior to 200~350 DEG C 2~4h of roasting, then at 600~ 700 DEG C of 6~8h of roasting to obtain the final product.
The low-carbon alcohols are one kind in ethyl alcohol, normal propyl alcohol, isopropanol, butanol and isobutanol.
The application of extracting flavonoids adminicle flavones in extraction persimmon leaves or Wild Jujube Leaf.
Using the method for the extraction adminicle extraction flavones, include the following steps: 1)Persimmon leaves or Wild Jujube Leaf are natural It dries, crush, be sieved, drying;2)By step 1)Gained ovendry power, extracting flavonoids adminicle and ethyl alcohol mixing using hot formulation or Multistage microwave amplifier, cooling are filtered to remove insoluble matter and concentrate removing ethyl alcohol.
Step 1)In, cross 40~60 mesh sieve, 60~80 DEG C of drying.
When being extracted using hot formulation:The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g:(0.5~0.8) g:(10~12)Ml, Extracting temperature are 50~60 DEG C, and extraction time is 1~1.5h, and the concentration of volume percent of the ethyl alcohol is 60%~75%.
During using multistage microwave amplifier:The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g:(0.2~0.3) g:(1.2~2.0)Ml, extraction time be 1~2 min, 150~200W of microwave power, the concentration of volume percent of ethyl alcohol used It is 55%~70%.
During using ultrasonic wave extraction:The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g:(0.3~0.5) g:(2.1~3.5)Ml, 30~45 DEG C of 10~15min of ultrasound, frequency 40KHz, the concentration of volume percent of ethyl alcohol used is 50% ~75%.
In the extraction adminicle of the present invention, selected four kinds of components are non-toxic, and safety is good, at low cost, and selected Four kinds of components are inorganic matter, and using water phase or the extracting method of organic phase, four kinds of components will not be dissolved into solvent In, can ensure that active ingredient and the separation of residue and the adminicle can be realized by simple filtration during post processing in this way.
Moreover, during using extracting flavonoids adminicle of the present invention extraction flavones, since flavones is hydroxyl and carbonyl Class compound,
Selected nanometer hydroxyapatite and nano-silica surface is respectively provided with a large amount of activity hydroxy, the two with solvent Collective effect under, Flavonoid substances " absorption " to the Nanosurface and solvent in plant can be had an effect, compared to molten Agent is directly extracted, and the two provides the effect of " channel " or " bridge ", improves recovery rate, and practice have shown that, when the two press than Example collocation uses, and extraction effect is more preferable;Simultaneously as its design feature, can opposite " selectivity " to Flavonoid substances into Row major adsorbs, and compared with the prior art, can higher improve flavones content in extract.
Beta-alumina in the present invention has complex porous structure, increases specific surface area(Contact area), in the present invention In work
With being:So that extraction adminicle, flavones have the contact of more depth with Extraction solvent, further promote extraction effect;And Nano-titanium dioxide then primarily serves the effect for providing structural support, is equivalent to carrier, it is ensured that the physics of the adminicle and change Learn the stabilization of structure.
In the preparation of extracting flavonoids adminicle:First nanometer hydroxyapatite and nano silicon dioxide are handled respectively with alcohol, Both regular surface hydroxyl, optimizes surface texture;Add in the side of temperature programming using the present invention after remaining two kinds of component Formula is roasted so that the overall structure of the adminicle is more stablized, the effect more long stable effect of assisted extraction, and is conducive to Its repeatable usability.
Compared with prior art, the present invention has the following advantages:
1st, extracting flavonoids adminicle component of the invention is simple, non-toxic, safety, prepares simply, at low cost;
2nd, comparison is found, when addition present invention extraction adminicle extracts, extract obtained yield is high, brass in extract Content it is high;
3rd, aftertreatment technology is simple and convenient, is directly filtered after extraction, and the residue for extracting adminicle and extract passes through Calcining can recycling after removing residue.
Specific embodiment
With specific embodiment, the invention will be further described below.
Embodiment 1
A kind of plant extract flavones extraction adminicle, is made of the raw material of following parts by weight:1 part of nanometer hydroxyapatite, receives .8 parts of silica 1 of rice, 4 parts of beta-alumina, 4 parts of nano-titanium dioxide.
The plant extract flavones preparation method of extraction adminicle, is made by following steps:
A)Nanometer hydroxyapatite is placed in low-carbon alcohols(Ethyl alcohol)Middle boiling reflux 3h, adds nano silicon dioxide, boils back 5h is flowed, concentration removing low-carbon alcohols after cooling;
B)Add in beta-alumina, nano-titanium dioxide grinding, prior to 200 DEG C roasting 4h roast 6h then at 600 DEG C to obtain the final product.
By the application of extracting flavonoids adminicle flavones in persimmon leaves are extracted.
Using the method for the extraction adminicle extraction flavones, include the following steps:
1)Persimmon leaves naturally dry crushes, and crosses 40 mesh sieve, 60 DEG C of drying;
2)By step 1)Gained ovendry power, extracting flavonoids adminicle and ethyl alcohol mixing use hot formulation or multistage microwave amplifier, cool down, It is filtered to remove insoluble matter and concentrates and remove ethyl alcohol;Cooled and filtered removes insoluble matter, and concentration removes ethyl alcohol.
In the present embodiment, extracted using hot formulation:The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g: 0.5g:10ml, Extracting temperature are 50 DEG C, extraction time 1h.The concentration of volume percent of the ethyl alcohol is 60%.
Embodiment 2
A kind of plant extract flavones extraction adminicle, is made of the raw material of following parts by weight:1 part of nanometer hydroxyapatite, receives .5 parts of silica 1 of rice, 3 parts of beta-alumina, 3 parts of nano-titanium dioxide.
The plant extract flavones preparation method of extraction adminicle, is made by following steps:A)By nano-hydroxy Apatite is placed in low-carbon alcohols(Normal propyl alcohol)Middle boiling reflux 4h, adds nano silicon dioxide, and boiling reflux 6h is concentrated after cooling Remove low-carbon alcohols;
B)Add in beta-alumina, nano-titanium dioxide grinding, prior to 350 DEG C roasting 2h roast 8h then at 700 DEG C to obtain the final product.
By the application of extracting flavonoids adminicle flavones in extraction persimmon leaves or Wild Jujube Leaf.
Using the method for the extraction adminicle extraction flavones, include the following steps:
1)Wild Jujube Leaf naturally dry crushes, and crosses 60 mesh sieve, 80 DEG C of drying;
2)By step 1)Gained ovendry power, extracting flavonoids adminicle and ethyl alcohol mixing use hot formulation or multistage microwave amplifier, cool down, It is filtered to remove insoluble matter and concentrates and remove ethyl alcohol;Cooled and filtered removes insoluble matter, and concentration removes ethyl alcohol.
In the present embodiment, using multistage microwave amplifier:The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g: 0.2g:1.2ml, extraction time are 1 min, microwave power 150W.The concentration of volume percent of ethyl alcohol used is 55%.
Embodiment 3
A kind of plant extract flavones extraction adminicle, is made of the raw material of following parts by weight:1 part of nanometer hydroxyapatite, receives 2 parts of silica of rice, 5 parts of beta-alumina, 5 parts of nano-titanium dioxide.
The plant extract flavones is used to the preparation method of extraction adminicle, with embodiment 1.
Using the method for described extraction adminicle extraction flavones, with embodiment 1, the difference lies in:Using hot formulation Extraction:The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g: 0.8g:12ml, Extracting temperature are 60 DEG C, extraction Time is 1.5h.The concentration of volume percent of the ethyl alcohol is 75%.
Embodiment 4
A kind of plant extract flavones extraction adminicle and preparation method thereof, with embodiment 2.
When using it for extraction flavones, with embodiment 2, the difference lies in using multistage microwave amplifier:Ovendry power, flavones The mixed proportion for extracting adminicle and ethyl alcohol is 1g: 0.3g:2.0ml, extraction time are 2 min, microwave power 200W.It is used The concentration of volume percent of ethyl alcohol is 70%.
Embodiment 5
A kind of plant extract flavones extraction adminicle and preparation method thereof, with embodiment 2.
When using it for extraction flavones, with embodiment 2, the difference lies in using ultrasonic wave extraction:Ovendry power, flavones The mixed proportion for extracting adminicle and ethyl alcohol is 1g:0.3g:2.1ml, 45 DEG C of ultrasound 15min, frequency 40KHz, ethyl alcohol used Concentration of volume percent be 50%.
Embodiment 6
A kind of plant extract flavones extraction adminicle and preparation method thereof, with embodiment 1.
When using it for extraction flavones, with embodiment 1, the difference lies in using ultrasonic wave extraction:Ovendry power, flavones The mixed proportion for extracting adminicle and ethyl alcohol is 1g:0.5g:3.5ml, 30 DEG C of ultrasounds 10min, frequency 40KHz, ethyl alcohol used Concentration of volume percent is 75%.
Contrast test
To show effect of the present invention, respectively according to the extracting factor in embodiment 1-6, take and do not add extraction adminicle Mode is tested, and is denoted as control group 1-6 respectively, is measured in embodiment 1-6 and control group 1-6 extracts using spectrophotometry Flavones content(Using rutin standard body as standard items during test).Table 1 is crude extract in embodiment 1-6 and control group 1-6 Brass content and extract yield.
Table 1 is the brass content and extract yield of crude extract in embodiment 1-6 and control group 1-6
As shown in Table 1, when addition present invention extraction adminicle carries out extracting flavonoids, the flavones that can significantly improve crude extract contains Amount and extract yield.

Claims (9)

1. a kind of plant extract flavones extraction adminicle, which is characterized in that be made of the raw material of following parts by weight:Nano-hydroxy 1 part of apatite, 1.5~2 parts of nano silicon dioxide, 3~5 parts of beta-alumina, 3~5 parts of nano-titanium dioxide.
2. the plant extract flavones described in claim 1 preparation method of extraction adminicle, which is characterized in that by following steps It is made:A)Nanometer hydroxyapatite is placed in 3~4 h of boiling reflux in low-carbon alcohols, adds nano silicon dioxide, boiling reflux 5~6 h, concentration removing low-carbon alcohols after cooling;B)Add in beta-alumina, nano-titanium dioxide grinding, prior to 200~350 DEG C roastings Burn 2~4h, then at 600~700 DEG C of 6~8h of roasting to obtain the final product.
3. the plant extract flavones as claimed in claim 2 preparation method of extraction adminicle, which is characterized in that the low-carbon Alcohol is one kind in ethyl alcohol, normal propyl alcohol, isopropanol, butanol and isobutanol.
4. plant extract flavones described in claim 1 with extraction adminicle in extraction persimmon leaves or Wild Jujube Leaf flavones should With.
5. utilize the method for extraction adminicle extraction flavones described in claim 1, which is characterized in that include the following steps:1) Persimmon leaves or Wild Jujube Leaf naturally dry crush, and are sieved, drying;2)By step 1)Gained ovendry power, extracting flavonoids adminicle and second Alcohol mixing is filtered to remove insoluble matter and is concentrated removing ethyl alcohol using hot formulation, supercritical ultrasonics technology or multistage microwave amplifier, cooling.
6. the method for extraction adminicle extraction flavones as claimed in claim 5, which is characterized in that step 1)In, cross 40~60 Mesh sieves, 60~80 DEG C of drying.
7. the method for extraction adminicle extraction flavones as claimed in claim 5, which is characterized in that during using the extraction of hot formulation: The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g:(0.5~0.8)g:(10~12)Ml, Extracting temperature 50 ~60 DEG C, extraction time is 1~1.5h, and the concentration of volume percent of the ethyl alcohol is 60%~75%.
8. the method for extraction adminicle extraction flavones as claimed in claim 5, which is characterized in that during using multistage microwave amplifier: The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g:(0.2~0.3)g:(1.2~2.0)Ml, extraction time be 1~2 min, 150~200W of microwave power, the concentration of volume percent of ethyl alcohol used is 55%~70%.
9. the method for extraction adminicle extraction flavones as claimed in claim 5, which is characterized in that during using ultrasonic wave extraction: The mixed proportion of ovendry power, extracting flavonoids adminicle and ethyl alcohol is 1g:(0.3~0.5)g:(2.1~3.5)Ml, 30~45 DEG C 10~15min of ultrasound, frequency 40KHz, the concentration of volume percent of ethyl alcohol used is 50%~75%.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109370251A (en) * 2018-11-12 2019-02-22 苏州经贸职业技术学院 A kind of high efficiency extraction technique of vegetable dyeing agent
CN111617132A (en) * 2020-06-12 2020-09-04 西藏天虹科技股份有限责任公司 Tibetan capillary artemisia extract and preparation method thereof
CN112006996A (en) * 2020-09-01 2020-12-01 江西纳弗堂制药有限公司 Quick production method of traditional Chinese medicine formula granules
CN112137018A (en) * 2020-09-09 2020-12-29 广东都市菜族农业科技有限公司 Noodles containing purple Chinese yam extract and preparation method thereof
US20230200421A1 (en) * 2021-12-27 2023-06-29 Wude Mao Method for preparing persimmon leaf extract

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Publication number Priority date Publication date Assignee Title
CN101016287A (en) * 2007-02-12 2007-08-15 西北农林科技大学 Method of extracting flavone from cabbage leaf
CN101497003A (en) * 2009-01-24 2009-08-05 大连理工大学 Multifunctional photocatalysis composite ceramic separation membrane as well as preparation method and use thereof
CN102719116A (en) * 2012-05-24 2012-10-10 同济大学 Preparation method of hydroxyapatite carrying nanometer titanium dioxide
CN104001471A (en) * 2014-06-13 2014-08-27 淮海工学院 Preparation method of silicon dioxide immobilized hydroxyapatite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016287A (en) * 2007-02-12 2007-08-15 西北农林科技大学 Method of extracting flavone from cabbage leaf
CN101497003A (en) * 2009-01-24 2009-08-05 大连理工大学 Multifunctional photocatalysis composite ceramic separation membrane as well as preparation method and use thereof
CN102719116A (en) * 2012-05-24 2012-10-10 同济大学 Preparation method of hydroxyapatite carrying nanometer titanium dioxide
CN104001471A (en) * 2014-06-13 2014-08-27 淮海工学院 Preparation method of silicon dioxide immobilized hydroxyapatite material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109370251A (en) * 2018-11-12 2019-02-22 苏州经贸职业技术学院 A kind of high efficiency extraction technique of vegetable dyeing agent
CN111617132A (en) * 2020-06-12 2020-09-04 西藏天虹科技股份有限责任公司 Tibetan capillary artemisia extract and preparation method thereof
CN111617132B (en) * 2020-06-12 2022-01-04 西藏天虹科技股份有限责任公司 Tibetan capillary artemisia extract and preparation method thereof
CN112006996A (en) * 2020-09-01 2020-12-01 江西纳弗堂制药有限公司 Quick production method of traditional Chinese medicine formula granules
CN112137018A (en) * 2020-09-09 2020-12-29 广东都市菜族农业科技有限公司 Noodles containing purple Chinese yam extract and preparation method thereof
US20230200421A1 (en) * 2021-12-27 2023-06-29 Wude Mao Method for preparing persimmon leaf extract

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