CN110101683A - The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf - Google Patents
The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf Download PDFInfo
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- CN110101683A CN110101683A CN201910360827.6A CN201910360827A CN110101683A CN 110101683 A CN110101683 A CN 110101683A CN 201910360827 A CN201910360827 A CN 201910360827A CN 110101683 A CN110101683 A CN 110101683A
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- flavonoid component
- olive leaf
- slow release
- nanometer particle
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/63—Oleaceae (Olive family), e.g. jasmine, lilac or ash tree
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/513—Organic macromolecular compounds; Dendrimers
- A61K9/5146—Organic macromolecular compounds; Dendrimers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, polyamines, polyanhydrides
- A61K9/5153—Polyesters, e.g. poly(lactide-co-glycolide)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/513—Organic macromolecular compounds; Dendrimers
- A61K9/5161—Polysaccharides, e.g. alginate, chitosan, cellulose derivatives; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5192—Processes
Abstract
The present invention provides a kind of preparation methods of flavonoid component slow release nanometer particle in olive leaf.Preparation step is as follows: a) dry, pulverize olive leaf at 50-60 DEG C to partial size is 60-100 mesh olive leaf fine powder;B) olive leaf fine powder is extracted using alkaline alcohol solution, it is low-temperature defatted;C) dynamic surface adsorption and purification, dry flavonoid component;D) above-mentioned flavonoid component is mixed with embedded material and is dissolved in organic solvent and obtains mixed solution, be passed through in crystalization in supercritical fluid kettle, form nano controlled-release particle, collecting nanoparticle is flavonoid component slow release nanometer particle.This method mainly enters flavonoid component in crystallization kettle after molten altogether with embedded material mix with supercritical fluid, moment formation nanoparticle.It is formed by outside flavonoid component slow release nanometer particle and is wrapped up by embedded material, be conducive to the slow releasing function of biological utilisation process, and availability is high, has no toxic side effect.
Description
Technical field
The present invention relates to pharmaceutical technology fields, and in particular to the preparation of flavonoid component slow release nanometer particle in a kind of olive leaf
Method.
Background technique
Olive (Olea europaea L.) is Oleaceae (Oleaceae), Olea (Olea) plant, olive
Chemical component in leaf includes secoiridoid, flavonoids, free alcohol, sterol, alkanes and volatile component etc., wherein yellow
Ketone compounds are one of the main actives in olive growing leaves.Studies have shown that olive leaf flavonoids have very strong antioxygen
Change activity, may replace chemical preservative for food fresh keeping, foreign countries have been widely used in cosmetics, food and drug.In addition,
After olive introduces China, the large-scale planting base for relatively having scale is had already appeared in some areas, but mainly utilize its fruit, and
A large amount of olive leaves are discarded, and are resulted in waste of resources.For the current situation of the current olive in China, added using the leaf of olive
Work bioactive substance obtains leaf extract especially with the discarded olive leaf of trimming, it will greatly improve olive
Economic value, make contributions for human health, thus, from olive growing leaves extract separating flavone class compound have important meaning
Justice.
The extraction separation method of olive leaf flavonoids reported at present include organic solvent extractionprocess, ultrasonic wave auxiliary mention
It follows the example of, microwave-assisted, supercritical fluid extraction and absorption method etc., mostly there is complex process, place for these methods
The disadvantages such as reason amount is small, equipment requirement is high, Extracting temperature is high, extraction time is long, solvent processing is troublesome, yield is low.It is used as medicine simultaneously
Powder is beaten with position convection drying and obtains that raw material bioavilability is not high, and solubility is lower, absorbs slow, is easy the pH value by environment
Influence causes to degrade.In addition, conventional method forms the core material composition that nanoparticle mostly uses polymerizable vinyl monomer
Carry out suspension polymerisation and formed, for this method there are inclusion rate is not high, the microspherulite diameter of generation is larger, be easy breakage, technique and
The problems such as energy consumption is higher.
Summary of the invention
Technical problems to be solved: the object of the present invention is to provide flavonoid component slow release nanometer particles in a kind of olive leaf
Flavonoid component is entered in crystallization kettle after molten altogether with embedded material and is mixed with supercritical fluid by preparation method, and moment is formed
Nanoparticle.It is formed by outside flavonoid component slow release nanometer particle and is wrapped up by embedded material, be conducive to biological utilisation process
Slow releasing function, and availability is high, has no toxic side effect.
A kind of technical solution: the preparation method of flavonoid component slow release nanometer particle in olive leaf, comprising the following steps:
A) dry, pulverize olive leaf at 50-60 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) olive leaf fine powder is extracted using alkaline alcohol solution, it is low-temperature defatted;
C) dynamic surface adsorption and purification, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with embedded material and is dissolved in organic solvent and obtains mixed solution, be passed through crystalization in supercritical fluid kettle
In, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle.
Further, the step b) neutral and alkali alcohol is ethyl alcohol or methanol, and concentration is that 40 ~ 70%, pH is 8 ~ 10, extracts temperature
Degree is 70 ~ 90 DEG C, and extraction time is 1.5 ~ 2h.
Further, low-temperature defatted in the step b) that degreasing and wax, active carbon are removed using active carbon combination
For particle or powder, skimming temp is 4 ~ 12 DEG C, degreasing time is 8 ~ for 24 hours.
Further, dynamic surface adsorbent material is in macroreticular resin AB-8, D101 or HPD300 in the step c)
One or more, eluent are 10% ammonia spirit.
Further, eluent basic anhydride aluminium is purified, and basic anhydride are 100 ~ 200 mesh.
Further, in the step d) embedded material be one or more of polylactic acid or ethyl cellulose, it is organic
Solvent is one or more of ethyl acetate, methylene chloride, chloroform.
Further, super-critical crystallization kettle condition in the step d): medium CO2Or N2, pressure is 8 ~ 20MPa, temperature
It is 15 ~ 35 DEG C, solution flow velocity is 0.5 ~ 2ml/min.
Further, flavonoid component mass fraction is 0.5 ~ 2% in mixed solution in the step d), embedded material concentration
It is 1 ~ 3%, the diameter of nano particles of formation is distributed in 500 ~ 15000nm.
The utility model has the advantages that
It mixes 1. the method for the present invention enters flavonoid component in crystallization kettle after molten altogether with embedded material with supercritical fluid, wink
Between form nanoparticle.
2. the extracted flavonoid component content of the method for the present invention is greater than 85%, prepared flavonoid component slow release nanometer particle
Diameter is distributed in 500 ~ 15000nm.
3. wrapping up outside the flavonoid component slow release nanometer particle of the method for the present invention preparation by embedded material, be conducive to biology
Using the slow releasing function of process, and availability is high, has no toxic side effect.
Specific embodiment
Embodiment 1
The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf, comprising the following steps:
A) dry, pulverize olive leaf at 50 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) ethyl alcohol for using concentration to be 8 for 40%, pH extracts, and Extracting temperature is 70 DEG C, extraction time 1.5h, using work
Property charcoal particle combination remove degreasing and wax, skimming temp be 4 DEG C, degreasing time 8h;
C) dynamic surface adsorption and purification, dynamic surface adsorbent material are macroreticular resin AB-8, and eluent is 10% ammonia spirit, are washed
De- liquid basic anhydride aluminium purify, and basic anhydride are 100 ~ 200 mesh, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with polylactic acid and is dissolved in ethyl acetate and obtains mixed solution, be passed through crystalization in supercritical fluid kettle
In, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle, wherein flavones in mixed solution
Constituent mass score is 0.5%, and embedded material concentration is 1%, super-critical crystallization kettle condition: medium CO2, pressure 8MPa, temperature
Degree is 15 DEG C, and solution flow velocity is 0.5ml/min.
Extracted flavonoid component content is 85.7%, and prepared flavonoid component slow release nanometer particle diameter is distributed in 700
~15000nm。
Embodiment 2
The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf, comprising the following steps:
A) dry, pulverize olive leaf at 55 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) methanol for using concentration to be 9 for 50%, pH extracts, and Extracting temperature is 75 DEG C, extraction time 2h, using activity
Carbon powder combination removes degreasing and wax, and skimming temp is 6 DEG C, degreasing time 12h;
C) dynamic surface adsorption and purification, dynamic surface adsorbent material are macroreticular resin D101, and eluent is 10% ammonia spirit, are washed
De- liquid basic anhydride aluminium purify, and basic anhydride are 100 ~ 200 mesh, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with ethyl cellulose and is dissolved in methylene chloride and obtains mixed solution, be passed through crystalization in supercritical fluid
In kettle, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle, wherein yellow in mixed solution
Ketone constituent mass score is 1%, and embedded material concentration is 1.5%, super-critical crystallization kettle condition: medium N2, pressure 11MPa,
Temperature is 20 DEG C, and solution flow velocity is 1ml/min.
Extracted flavonoid component content is 86.1%, and prepared flavonoid component slow release nanometer particle diameter is distributed in 550
~14000nm。
Embodiment 3
The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf, comprising the following steps:
A) dry, pulverize olive leaf at 55 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) ethyl alcohol for using concentration to be 9 for 55%, pH extracts, and Extracting temperature is 80 DEG C, extraction time 1.5h, using work
Property charcoal particle combination remove degreasing and wax, skimming temp be 8 DEG C, degreasing time 16h;
C) dynamic surface adsorption and purification, dynamic surface adsorbent material are macroreticular resin HPD300, and eluent is 10% ammonia spirit,
Eluent basic anhydride aluminium is purified, and basic anhydride are 100 ~ 200 mesh, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with polylactic acid and is dissolved in chloroform and obtains mixed solution, be passed through crystalization in supercritical fluid kettle
In, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle, wherein flavones in mixed solution
Constituent mass score is 1.3%, and embedded material concentration is 2%, super-critical crystallization kettle condition: medium CO2, pressure 14MPa, temperature
Degree is 25 DEG C, and solution flow velocity is 1.5ml/min.
Extracted flavonoid component content is 86.5%, and prepared flavonoid component slow release nanometer particle diameter is distributed in 500
~13000nm。
Embodiment 4
The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf, comprising the following steps:
A) dry, pulverize olive leaf at 55 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) methanol for using concentration to be 9 for 60%, pH extracts, and Extracting temperature is 85 DEG C, extraction time 2h, using activity
Charcoal particle combination removes degreasing and wax, and skimming temp is 10 DEG C, degreasing time 20h;
C) dynamic surface adsorption and purification, dynamic surface adsorbent material are macroreticular resin AB-8, and eluent is 10% ammonia spirit, are washed
De- liquid basic anhydride aluminium purify, and basic anhydride are 100 ~ 200 mesh, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with ethyl cellulose and is dissolved in ethyl acetate and obtains mixed solution, be passed through crystalization in supercritical fluid
In kettle, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle, wherein yellow in mixed solution
Ketone constituent mass score is 1.5%, and embedded material concentration is 2.5%, super-critical crystallization kettle condition: medium N2, pressure is
17MPa, temperature are 30 DEG C, and solution flow velocity is 1.5ml/min.
Extracted flavonoid component content is 86.3%, and prepared flavonoid component slow release nanometer particle diameter is distributed in 500
~14000nm。
Embodiment 5
The preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf, comprising the following steps:
A) dry, pulverize olive leaf at 60 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) methanol for using concentration to be 10 for 70%, pH extracts, and Extracting temperature is 90 DEG C, extraction time 1.5h, using work
Property carbon powder combination remove degreasing and wax, skimming temp be 12 DEG C, degreasing time be for 24 hours;
C) dynamic surface adsorption and purification, dynamic surface adsorbent material are macroreticular resin HPD300, and eluent is 10% ammonia spirit,
Eluent basic anhydride aluminium is purified, and basic anhydride are 100 ~ 200 mesh, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with polylactic acid and is dissolved in chloroform and obtains mixed solution, be passed through crystalization in supercritical fluid kettle
In, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle, wherein flavones in mixed solution
Constituent mass score is 2%, and embedded material concentration is 3%, super-critical crystallization kettle condition: medium CO2, pressure 20MPa, temperature
It is 35 DEG C, solution flow velocity is 2ml/min.
Extracted flavonoid component content is 86.1%, and prepared flavonoid component slow release nanometer particle diameter is distributed in 550
~14500nm。
Claims (8)
1. the preparation method of flavonoid component slow release nanometer particle in a kind of olive leaf, it is characterised in that: the following steps are included:
A) dry, pulverize olive leaf at 50-60 DEG C to partial size is 60-100 mesh olive leaf fine powder;
B) olive leaf fine powder is extracted using alkaline alcohol solution, it is low-temperature defatted;
C) dynamic surface adsorption and purification, dry flavonoid component;
D) above-mentioned flavonoid component is mixed with embedded material and is dissolved in organic solvent and obtains mixed solution, be passed through crystalization in supercritical fluid kettle
In, nano controlled-release particle is formed, collecting nanoparticle is flavonoid component slow release nanometer particle.
2. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 1
In the step b) neutral and alkali alcohol is ethyl alcohol or methanol, and concentration is that 40 ~ 70%, pH is 8 ~ 10, and Extracting temperature is 70 ~ 90 DEG C, is mentioned
Taking the time is 1.5 ~ 2h.
3. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 1
In, in the step b) it is low-temperature defatted using active carbon combination remove degreasing and wax, active carbon be particle or powder,
Skimming temp be 4 ~ 12 DEG C, degreasing time be 8 ~ for 24 hours.
4. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 1
In dynamic surface adsorbent material is one or more of macroreticular resin AB-8, D101, HPD300, elution in the step c)
Liquid is 10% ammonia spirit.
5. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 4
In eluent basic anhydride aluminium is purified, and basic anhydride are 100 ~ 200 mesh.
6. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 1
In, in the step d) embedded material be one or more of polylactic acid or ethyl cellulose, organic solvent be ethyl acetate,
One or more of methylene chloride, chloroform.
7. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 2
In super-critical crystallization kettle condition in the step d): medium CO2Or N2, pressure is 8 ~ 20MPa, and temperature is 15 ~ 35 DEG C, solution
Flow velocity is 0.5 ~ 2ml/min.
8. the preparation method of flavonoid component slow release nanometer particle, feature exist in a kind of olive leaf according to claim 2
In flavonoid component mass fraction is 0.5 ~ 2% in mixed solution in the step d), and embedded material concentration is 1 ~ 3%, and formation is received
Rice corpuscles diameter is distributed in 500 ~ 15000nm.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1314146A (en) * | 2001-02-12 | 2001-09-26 | 孙传经 | Supercritical CO2 solvent-resistant device for producing nanometer material |
CN1397555A (en) * | 2002-09-03 | 2003-02-19 | 单树森 | Process for preparing superfine particles of ginkgolic flavone by supercritical crystallizing method |
CN102228514A (en) * | 2011-05-05 | 2011-11-02 | 陕西禾博天然产物有限公司 | Method for extracting oleuropein from olive leaves |
CN103211750A (en) * | 2012-01-20 | 2013-07-24 | 纳米及先进材料研发院有限公司 | Method of preparing soy isoflavone nanoparticles by precipitation with compressed antisolvent (PCA) using a supercritical fluid |
-
2019
- 2019-04-30 CN CN201910360827.6A patent/CN110101683A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1314146A (en) * | 2001-02-12 | 2001-09-26 | 孙传经 | Supercritical CO2 solvent-resistant device for producing nanometer material |
CN1397555A (en) * | 2002-09-03 | 2003-02-19 | 单树森 | Process for preparing superfine particles of ginkgolic flavone by supercritical crystallizing method |
CN102228514A (en) * | 2011-05-05 | 2011-11-02 | 陕西禾博天然产物有限公司 | Method for extracting oleuropein from olive leaves |
CN103211750A (en) * | 2012-01-20 | 2013-07-24 | 纳米及先进材料研发院有限公司 | Method of preparing soy isoflavone nanoparticles by precipitation with compressed antisolvent (PCA) using a supercritical fluid |
Non-Patent Citations (3)
Title |
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Application publication date: 20190809 |