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CN104042567A - Ampelopsin nano-micelle and application thereof - Google Patents

Ampelopsin nano-micelle and application thereof Download PDF

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Publication number
CN104042567A
CN104042567A CN201410249243.9A CN201410249243A CN104042567A CN 104042567 A CN104042567 A CN 104042567A CN 201410249243 A CN201410249243 A CN 201410249243A CN 104042567 A CN104042567 A CN 104042567A
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ampelopsin
nano
micelle
carrier
tumor
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CN201410249243.9A
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Inventor
黄仁杰
倪峰
狄万鹏
张月芬
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FUJIAN HEALTH COLLEGE
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FUJIAN HEALTH COLLEGE
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Priority to CN201410249243.9A priority Critical patent/CN104042567A/en
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Abstract

The invention discloses an ampelopsin nano-micelle and application thereof. The ampelopsin nano-micelle is prepared from a carrier and ampelopsin, wherein the carrier is a mixture of pluronic F127 and D-alpha-tocopheryl polyethylene glycol 1000 succinate; the feeding mass ratio of the ampelopsin to the carrier is (1:10)-(1:30); the feeding mass ratio of the pluronic F127 to the D-alpha-tocopheryl polyethylene glycol 1000 succinate in the carrier is (1:3)-(1:10). The ampelopsin nano-micelle can be used for remarkably improving the solubility of ampelopsin, has a higher encapsulation efficiency and a certain sustained-release effect, can be applied to injection, and can be used for remarkably improving the treatment effect when being used for treating patients with prostatic cancer.

Description

A kind of ampelopsin nano-micelle and application thereof
Technical field
The invention belongs to field of pharmaceutical preparations, relate to a kind of ampelopsin nano-micelle and application thereof.
Background technology
Ampelopsin has another name called dihydromyricetin, and this compound is separated obtaining the leaf of A. Meliaefolia A.Meliaefolia first in 1940 from Vitaceae ampelopsis fujian tea with Kubota by Kotake, called after ampelopsin.Ampelopsin has been proved to be antitumor, antioxidation, blood fat reducing, antiinflammatory, the effect such as antibacterial, but because its dissolubility is little, and may be through bacterial action and by metabolism in intestinal, so oral administration bioavailability is low.Separately, because dissolubility in its water is little, be unfavorable for making drug administration by injection form.These are all to affect the obstacle that it is applied clinically, and the Related product that yet there are no ampelopsin monomer is applied to clinical.Although there is bibliographical information (Ruan LP, Yu BY, et.al.Improving thesolubility of ampelopsin by solid dispersions and inclusion complexes.Journal ofPharmaceutical andBiomedical Analysis.2005,38 (3): 457-64) adopt the preparation techniques such as solid dispersions technique, cyclodextrin inclusion technique to improve the dissolubility of ampelopsin, but these methods exist complicated process of preparation, cost is high and can only solely improve dissolubility, and can not reach slow release and the object of injecting purposes.And adopt the reagent such as surfactant, ethanol, dimethyl sulfoxide to increase dissolubility, there is again the shortcoming that toxicity or zest are large.
Due to the existence of these problems, therefore, ampelopsin water solublity a kind ofly can be improved in the urgent need to developing in this area, can delay drug release again, extends biological half-life, improves a kind of novel ampelopsin induction system of curative effect.
Summary of the invention
The object of this invention is to provide a kind of ampelopsin nano-micelle, it can improve ampelopsin water solublity, can delay drug release again, extends biological half-life, and can improve curative effect.
Ampelopsin nano-micelle provided by the present invention, is prepared from by carrier and ampelopsin; Described carrier is the mixture of pluronic F127 and polyethylene glycol 1000 vitamin E succinate.
In above-mentioned ampelopsin nano-micelle, the mass ratio that feeds intake of ampelopsin and carrier is 1: 10 to 1: 30 (1: 10-30), is preferably 1: 20.
In above-mentioned carrier, the mass ratio that feeds intake of described pluronic F127 and polyethylene glycol 1000 vitamin E succinate is 1: 3 to 1: 10 (1: 3-10), be preferably 1: 8, described polyethylene glycol 1000 vitamin E succinate, is called for short TPGS 1000.
The preparation method of above-mentioned ampelopsin nano-micelle, comprise the steps: described ampelopsin and described carrier to be placed in container, add wherein again methanol, described paclitaxel and described carrier are dissolved in described methanol, remove again methanol and make the mixture of described paclitaxel and described carrier by rotary evaporation, form thin film (refinement explanation possibly here: " mixture is how can form thin film on container inner wall ") on described container inner wall, in described container, add purified water again, formed thin film on chamber wall is carried out to hydration process, obtain hydration process product, obtain described ampelopsin nano-micelle, the described methanol step of removing again can be by Rotary Evaporators vacuum, to remove methanol under preference temperature, or other this area routine is removed methanol measure and all can.
In the preparation method of above-mentioned ampelopsin nano-micelle, the method for described hydration process is for being equipped with container jolting 30min at 37 ℃ of described thin film and purified water, and described jolting can be ultrasound treatment patterns, or other this area conventional measure all can.
In the preparation method of above-mentioned ampelopsin nano-micelle, after described hydration process, hydration process product can also be carried out to the step of 0.1 μ m aperture membrane filtration.
The mean diameter of above-mentioned ampelopsin nano-micelle is 22.8 ± 0.5nm.
The polydispersity coefficient of the particle diameter of above-mentioned ampelopsin nano-micelle is all less than 0.2.
The Zeta potential of above-mentioned ampelopsin nano-micelle is-20.73mV.
In above-mentioned ampelopsin nano-micelle, the content of ampelopsin is 3.27 ± 0.12mg/ml.
The application of above-mentioned arbitrary described ampelopsin nano-micelle in the medicine that suppresses tumor in preparation also belongs to protection scope of the present invention.
In above-mentioned application, described inhibition tumor is for suppressing the propagation of tumor and/or the survival of inhibition tumor cell;
In above-mentioned application, the propagation that the propagation of described inhibition tumor is inhibition tumor cell and/or inhibition tumor sphere volume increase and/or promote disintegrating of tumor ball;
In above-mentioned application, described tumor is carcinoma of prostate; Described prostatic cell is prostate gland cancer cell PC-3, prostate gland cancer cell DU-145.
Beneficial effect of the present invention:
1) ampelopsin nano-micelle of the present invention, has improved 16 times of left and right by ampelopsin dissolubility in water, makes it can meet the requirement of daily drug administration by injection dosage.And preparation can cumulative release in 12h more than 80%, in the time of the release of prolong drug, can guarantee again the release completely of medicine, improve the therapeutic effect of medicine.
2) ampelopsin nano-micelle of the present invention, adopts two kinds of carrier materials to mix and uses, and improves envelop rate and the stability of medicine, and the drug resistance that can overcome medicine produces the outer row that can reduce again medicine in cell, gives full play to the therapeutical effect of medicine.
3) preparation of the present invention has good auxiliary therapeutic action to the disease of the serious harm human healths such as tumor, and particularly the therapeutic effect of carcinoma of prostate is obvious.
Accompanying drawing explanation
Fig. 1 describes ampelopsin nano-micelle transmission electron microscope scintigram.
Fig. 2 is the figure that describes the drug-eluting curve of ampelopsin nano-micelle in different medium.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.The experimental technique of unreceipted actual conditions in the following example, conventionally according to normal condition, or the condition of advising according to manufacturer.
embodiment 1
Precision takes TPGS respectively 10008g, pluronic F 1271g, ampelopsin 0.45g, be dissolved in appropriate methanol, by Rotary Evaporators vacuum, remove methanol at 37 ℃, in eggplant-shape bottle bottom and inwall form the uniform films of thin layer, the purified water that adds 50mL, aquation 30min in 37 ℃ of water-baths, sealing is placed in the about 6h of refrigerator, supersound process 10min, treat that thin film comes off completely, with the polycarbonate membrane difference filter 23 of 0.2 μ m, 0.1 μ m, obtain ampelopsin nano-micelle preparations successively, envelop rate is 80.1%.
embodiment 2
Precision takes TPGS respectively 10005g, pluronic F 1271g, ampelopsin 0.3g, be dissolved in appropriate methanol, by Rotary Evaporators vacuum, remove methanol at 37 ℃, in eggplant-shape bottle bottom and inwall form the uniform films of thin layer, the purified water that adds 50mL, aquation 30min in 37 ℃ of water-baths, sealing is placed in the about 6h of refrigerator, supersound process 10min, treat that thin film comes off completely, with the polycarbonate membrane difference filter 23 of 0.2 μ m, 0.1 μ m, obtain ampelopsin nano-micelle preparations successively, envelop rate is 74.9%.
embodiment 3
Precision takes TPGS respectively 10008g, pluronic F 1271g, ampelopsin 0.9g, be dissolved in appropriate methanol, by Rotary Evaporators vacuum, remove methanol at 37 ℃, in eggplant-shape bottle bottom and inwall form the uniform films of thin layer, the purified water that adds 50mL, aquation 30min in 37 ℃ of water-baths, sealing is placed in the about 6h of refrigerator, supersound process 10min, treat that thin film comes off completely, with the polycarbonate membrane difference filter 23 of 0.2 μ m, 0.1 μ m, obtain ampelopsin nano-micelle preparations successively, envelop rate is 70.7%.
embodiment 4
Precision takes TPGS respectively 10008g, pluronic F 1271g, ampelopsin 0.6g, be dissolved in appropriate methanol, by Rotary Evaporators vacuum, remove methanol at 37 ℃, in eggplant-shape bottle bottom and inwall form the uniform films of thin layer, the purified water that adds 50mL, aquation 30min in 37 ℃ of water-baths, sealing is placed in the about 6h of refrigerator, supersound process 10min, treat that thin film comes off completely, with the polycarbonate membrane difference filter 23 of 0.2 μ m, 0.1 μ m, obtain ampelopsin nano-micelle preparations successively, envelop rate is 72.7%.
embodiment 5
Use the method for preparing nano-micelle in above-described embodiment to make pastille nano-micelle, then by this pastille nano-micelle fill in ampoule bottle, through lyophilization, process, sealing, obtains ampelopsin nano-micelle lyophilized injectable powder.
embodiment 6 ampelopsin nano-micelle Morphological Characterizations
Get the ampelopsin nano-micelle that appropriate embodiment 1 makes, after dilution, with Nicomp 380/ZLS laser particle size and current potential, survey instrument and measure particle diameter and distribution and Zeta potential.Experimental result shows that the mean diameter of ampelopsin nano-micelle is at 22.8 ± 0.5nm, and polydispersity coefficient is all less than 0.2, shows that dispersion is good, and Zeta potential is-20.73mV.
Get the ampelopsin nano-micelle that embodiment 1 makes appropriate, use phosphotungstic acid negative staining, drip on the Electronic Speculum copper mesh of plated film, after drying, be placed in the form of electric Microscopic observation nanoparticle.As shown in Figure 1, visible nano-micelle is spherical, outward appearance rounding, and uniform particle diameter, size is consistent with the measurement result of laser particle analyzer.
embodiment 7 dissolubility are investigated
The ampelopsin nano-micelle lyophilized powder respectively embodiment 1 being made adds in certain water gaging, and in 25 ℃ of water bath with thermostatic control agitators, jolting is to dissolution equilibrium.Sampling is appropriate respectively, through 0.22 μ m microporous filter membrane, filters, and is placed in 10mL volumetric flask and adds methanol constant volume.By HPLC method, measure its peak area, by external standard counter point, difference calculated equilibrium dissolubility.Result demonstration, the ampelopsin dissolubility in ampelopsin nano-micelle of the present invention is by 0.4861 mgml of routine -1be increased to 7.7444mgml -1, increased by 16 times.
embodiment 8 ampelopsin nano-micelle extracorporeal releasing experiments
Essence is got bag filter that 2mL ampelopsin nano micellar solution that embodiment 1 makes is placed in treated mistake (in (8000-14000 dalton) respectively, after being tightened, puts into bag mouth the beaker of the different release medium (simulated gastric fluid, purified water, pH6.8 phosphate-buffered salt and pH7.4 cattle fetal blood are clear) that 200mL is housed, being placed in 37 ℃ of constant temperature oscillators shakes, regularly draw dialysis solution 1mL, simulated gastric fluid, purified water, phosphate-buffered salt and the cattle fetal blood of adding equivalent clear simultaneously.Adopt HPLC method to measure ampelopsin content, and calculate accumulative total release rate, its release profiles is shown in Fig. 2.As shown in the figure, 12h can more than 80% medicine of cumulative release in 4 kinds of different mediums for ampelopsin nano-micelle, and has certain slow-release capability.
embodiment 9 ampelopsin nano-micelle In Vitro Anti carcinoma of prostate activity experiments
1. ampelopsin nano-micelle In Vitro Anti carcinoma of prostate is active
1.1 experiment groupings
(1) the ampelopsin nano-micelle group that embodiment 1 makes is (containing ampelopsin, F127+TPGS1000; Medicine and total carrier are than being 1:20, and F127 and TPGS1000 ratio are 8:1): with ampelopsin content meter, establish respectively 25,50,100,150,200,250ug/ml Concentraton gradient.
(2) the naked medicine group of ampelopsin (only containing ampelopsin crude drug): establish 25,50,100,150,200,250ug/ml Concentraton gradient.
(4) blank group (not adding any medicine, cell normal growth): add isopyknic PBS or culture medium.
1.2 medicinal liquid preparations
(1) ampelopsin, with DMSO hydrotropy, is diluted to desired concn gradient (wherein DMSO concentration is not higher than 0.01%) by PBS or culture medium
(2) ampelopsin nano-micelle, directly with PBS preparation, is crossed the degerming of 0.1um filter membrane, with PBS or culture medium, is diluted to desired concn gradient.
1.3 mtt assay
The take the logarithm prostate gland cancer cell of trophophase, trypsinization counting, makes the single cell suspension of suitable concentration.96 orifice plates are around filled with PBS, and zone line is by the cell of every hole 180ul suspension inoculation suitable number.Cell attachment after cultivation 24h, adds the medicine of Concentraton gradient, and establishes blank, continues to cultivate 72h.After 72h, inhale and abandon culture fluid, add the MTT liquid of 5mg/ml, 20ul/ hole.Continue to hatch after 4h, carefully abandon supernatant, add DMSO dissolving crystallized, 150ul/ hole.Concussion 10min, upper microplate reader is measured OD in 570nm place.Be calculated as follows survival rate: survival rate (%)=(experimental group OD/ matched group OD) * 100%.
2 experimental results
The impact of 2.1 ampelopsin nano-micelles on prostate gland cancer cell PC-3 growth
The survival rate of PC-3 cell after table 1. variable concentrations ampelopsin and nano-micelle intervention thereof
Result shows, ampelopsin nano-micelle suppresses prostate gland cancer cell PC-3 successful and is better than ampelopsin raw material group, and both have significant difference (p<0.0l).
The impact of 2.2 ampelopsin nano-micelles on prostate gland cancer cell DU-145 growth
The survival rate of DU145 cell after table 2 variable concentrations ampelopsin and nano-micelle intervention thereof
Result shows, ampelopsin nano-micelle suppresses prostate gland cancer cell DU-145 successful and is better than ampelopsin raw material group, and both have significant difference (p<0.0l).
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in description and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the general concept that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend of describing.

Claims (10)

1. an ampelopsin nano-micelle, is prepared from by carrier and ampelopsin; Described carrier is the mixture of pluronic F127 and polyethylene glycol 1000 vitamin E succinic acid ester;
The mass ratio that feeds intake of described ampelopsin and carrier is 1: 10 to 1: 30;
In described carrier, the mass ratio that feeds intake of pluronic F127 and polyethylene glycol 1000 vitamin E succinate is 1: 3 to 1: 10.
2. according to the ampelopsin nano-micelle described in claim 1, it is characterized in that: the mass ratio that feeds intake of described ampelopsin and carrier is 1: 20.
3. according to the ampelopsin nano-micelle described in claim 1, it is characterized in that:
In described carrier, the mass ratio that feeds intake of pluronic F127 and polyethylene glycol 1000 vitamin E succinate is 1: 8.
4. according to the ampelopsin nano-micelle described in claim 1 or 2 or 3, it is characterized in that: the mean diameter of described ampelopsin nano-micelle is 22.8 ± 0.5nm;
The polydispersity coefficient of the particle diameter of described ampelopsin nano-micelle is less than 0.2.
5. according to the ampelopsin nano-micelle described in claim 4, it is characterized in that: the Zeta potential of described ampelopsin nano-micelle is-20.73mV.
6. according to the ampelopsin nano-micelle described in claim 5, it is characterized in that: in described ampelopsin nano-micelle, the content of ampelopsin is 3.27 ± 0.12mg/ml.
7. the preparation method of the arbitrary described ampelopsin nano-micelle of claim 1-6, comprise the steps: the carrier of the ampelopsin of formula ratio and formula ratio to be placed in container, add wherein again methanol, ampelopsin and carrier are dissolved in methanol, by removing the step of methanol, make the mixture of ampelopsin and carrier on container inner wall, form thin film, in described container, add purified water again, formed thin film on container inner wall is carried out to hydration process, obtain hydration process product, obtain described ampelopsin nano-micelle.
8. according to the preparation method of the ampelopsin nano-micelle described in claim 7, it is characterized in that: the method for described hydration process is for being equipped with container jolting 30min at 37 ℃ of thin film and purified water.
9. the application of the arbitrary described ampelopsin nano-micelle of claim 1-6 in the medicine of preparation inhibition tumor.
10. according to the application described in claim 9, it is characterized in that: described inhibition tumor for suppress tumor propagation and/or
The survival of inhibition tumor cell;
And/or, the propagation that the propagation of described inhibition tumor is inhibition tumor cell and/or suppress that tumor sphere volume increases and/
Or promote disintegrating of tumor ball;
And/or described tumor is carcinoma of prostate; Described prostatic cell is prostate gland cancer cell PC-3, prostate gland cancer cell DU-145.
CN201410249243.9A 2014-06-07 2014-06-07 Ampelopsin nano-micelle and application thereof Pending CN104042567A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
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CN106750272A (en) * 2016-12-05 2017-05-31 福建卫生职业技术学院 A kind of water-soluble ampelopsin polymer
CN107019670A (en) * 2017-04-18 2017-08-08 国家纳米科学中心 A kind of nano-micelle pharmaceutical carrier based on vitamin e derivative, nano-micelle pharmaceutical composition and its preparation method and application
CN108014104A (en) * 2018-01-22 2018-05-11 青岛科技大学 A kind of Synergistic type dihydromyricetin soluble type compound and preparation method thereof
WO2019050969A1 (en) * 2017-09-06 2019-03-14 Prud'homme, Robert, K. Dihydromyricetin nanoparticle formulations
CN109568297A (en) * 2018-11-22 2019-04-05 福建中医药大学 A kind of dihydromyricetin solid lipid nano granule and preparation method
US11103461B2 (en) 2015-12-22 2021-08-31 The Trustees Of Princeton University Process for encapsulating soluble biologics, therapeutics, and imaging agents
US11554101B2 (en) 2014-06-24 2023-01-17 The Trustees Of Princeton University Process for encapsulating soluble biologics, therapeutics, and imaging agents
US11731099B2 (en) 2018-07-20 2023-08-22 The Trustees Of Princeton University Method for controlling encapsulation efficiency and burst release of water soluble molecules from nanoparticles and microparticles produced by inverse flash nanoprecipitation
US11737981B2 (en) 2017-09-12 2023-08-29 The Trustees Of Princeton University Cellulosic polymer nanoparticles and methods of forming them
US12186436B2 (en) 2018-07-19 2025-01-07 The Trustees Of Princeton University Triblock copolymer stabilizers for the formation of nanoparticles encapsulating soluble biologics, therapeutics, and imaging agents
US12343324B2 (en) 2018-11-14 2025-07-01 The Trustees Of Princeton University Dihydromyricetin hot melt extrusion formulations and methods for forming them
US12357582B2 (en) 2017-11-03 2025-07-15 The Trustees Of Princeton University Hydrophobic ion pairing and flash nanoprecipitation for formation of controlled-release nanocarrier formulations

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11554101B2 (en) 2014-06-24 2023-01-17 The Trustees Of Princeton University Process for encapsulating soluble biologics, therapeutics, and imaging agents
US11103461B2 (en) 2015-12-22 2021-08-31 The Trustees Of Princeton University Process for encapsulating soluble biologics, therapeutics, and imaging agents
CN106750272A (en) * 2016-12-05 2017-05-31 福建卫生职业技术学院 A kind of water-soluble ampelopsin polymer
CN106750272B (en) * 2016-12-05 2019-05-28 福建卫生职业技术学院 A kind of water solubility ampelopsin polymer
CN107019670B (en) * 2017-04-18 2020-06-16 国家纳米科学中心 Vitamin E derivative-based nano-micelle drug carrier, nano-micelle drug composition, and preparation method and application thereof
CN107019670A (en) * 2017-04-18 2017-08-08 国家纳米科学中心 A kind of nano-micelle pharmaceutical carrier based on vitamin e derivative, nano-micelle pharmaceutical composition and its preparation method and application
WO2019050969A1 (en) * 2017-09-06 2019-03-14 Prud'homme, Robert, K. Dihydromyricetin nanoparticle formulations
US11737981B2 (en) 2017-09-12 2023-08-29 The Trustees Of Princeton University Cellulosic polymer nanoparticles and methods of forming them
US12357582B2 (en) 2017-11-03 2025-07-15 The Trustees Of Princeton University Hydrophobic ion pairing and flash nanoprecipitation for formation of controlled-release nanocarrier formulations
CN108014104A (en) * 2018-01-22 2018-05-11 青岛科技大学 A kind of Synergistic type dihydromyricetin soluble type compound and preparation method thereof
US12186436B2 (en) 2018-07-19 2025-01-07 The Trustees Of Princeton University Triblock copolymer stabilizers for the formation of nanoparticles encapsulating soluble biologics, therapeutics, and imaging agents
US11731099B2 (en) 2018-07-20 2023-08-22 The Trustees Of Princeton University Method for controlling encapsulation efficiency and burst release of water soluble molecules from nanoparticles and microparticles produced by inverse flash nanoprecipitation
US12343324B2 (en) 2018-11-14 2025-07-01 The Trustees Of Princeton University Dihydromyricetin hot melt extrusion formulations and methods for forming them
CN109568297A (en) * 2018-11-22 2019-04-05 福建中医药大学 A kind of dihydromyricetin solid lipid nano granule and preparation method

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