CN103877625A - PLGA (poly(lactic-co-glycolic acid))/bletilla composite microsphere for embolism and preparation method thereof - Google Patents
PLGA (poly(lactic-co-glycolic acid))/bletilla composite microsphere for embolism and preparation method thereof Download PDFInfo
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- CN103877625A CN103877625A CN201410077732.0A CN201410077732A CN103877625A CN 103877625 A CN103877625 A CN 103877625A CN 201410077732 A CN201410077732 A CN 201410077732A CN 103877625 A CN103877625 A CN 103877625A
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Abstract
The invention relates to a PLGA (poly(lactic-co-glycolic acid))/bletilla composite microsphere for embolism and a preparation method thereof. The preparation method comprises the following steps: mixing a PLGA organic solution with a bletilla polysaccharide aqueous solution under an ultrasound condition, adding an ethylenediamine aqueous solution into the obtained emulsion, performing ultrasonic mixing continuously and bletilla polysaccharide crosslinking, dispersing the obtained water in oil mixed emulsion into a PVA (polyvinyl acetate) aqueous solution, stirring and emulsifying for 10-14 hours, volatizing an organic solvent, performing bletilla polysaccharide crosslinking and microsphere solidifying, washing with water and performing suction filtration, so that the PLGA/bletilla composite microsphere is obtained. Results show that the composite spheres with different grain diameters ranging from 50 microns to 1000 microns can be prepared under the condition of appropriate technological parameters, the spheres are regular, and the PLGA/bletilla composite microsphere is a novel microsphere preparation applicable to embolism and drug sustained release.
Description
Technical field
The invention belongs to macromolecular material and biomedical engineering field, be specifically related to a kind of thromboembolism PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere and preparation method thereof.
Background technology
Metastatic tumo(u)r is the high common disease of fatality rate in cancer patient, and excision is considered to current only effective Therapeutic Method completely, but only has 25% the patient treatment of can performing a surgical operation.Therefore,, in order to make can be suitable for the effective means of performing the operation or non-operative treatment being provided by tumor resection, interventional therapy is widely used in treating malignant tumor.Transcatheter arterial em-bolization is being used widely aspect treatment late tumor in recent years.Transcatheter arterial em-bolization is that conduit is inserted to tremulous pulse, the more required embolism materials of performing a surgical operation is transported to target organ or target tissue.The blood of the clogging target organ of embolism materials or target tissue supplies and supports confession, can play by embolus carrying medicament or nucleic the effect of further treatment simultaneously.The development of transcatheter arterial em-bolization makes microsphere be used widely as main thromboembolism preparation.
Biodegradable absorbable polymer polymer microsphere, as embolism materials time, in the process of its degraded and absorbed, anticancer effective component slowly can be released to tumor by local and maintain active drug concentration, not only can reduce the general toxic reaction of cancer therapy drug, can also optionally improve the drug level of tumor by local simultaneously, the therapeutic effect that strengthens chemotherapeutics and radiotherapy non-operative treatment, therefore, Biodegradable material obtains extensive concern in transcatheter arterial em-bolization.For adapting to the needs of different parts heterogeneity pathological changes, the research and development of novel embolizing material and application are always in exploring.
Poly(D,L-lactide-co-glycolide (PLGA) can biosynthesis, can adjust its degradation speed by adjusting ratio, is the controlled degradable biomaterial of a kind of degradation speed.The PLGA first Application of 20 century 70 synthetic, in the long-acting controlled release system of medicine, obtains U.S. FAD approval.Two kinds of product lactic acid after PLGA hydrolysis and hydroxyacetic acid, be the by-product of body metabolism approach, nontoxic to human-body safety, therefore PLGA biological safety is high, can, along with body metabolism, can there is not accumulating phenomenon in its repetitively administered, be a kind of well drug conveying carrier later in vivo.
Pseudobulbus Bletillae polysaccharose is to extract through certain technique the polysaccharide obtaining from Pseudobulbus Bletillae (Rhizoma Bletillae) medical material, by glucose and mannose (1:4) with β glycosidic bond a kind of mannosym that is polymerized, in vivo can biodegradation, be hydrolyzed to CO through liver metabolism
2and H
2o.The contained lymphatic temperament of the Pseudobulbus Bletillae (Rhizoma Bletillae) itself is a kind of broad-spectrum anti-tumor composition, the aldehyde radical that it is free and alpha-alcohol ketone can or disturb the intermediation of heparinoid proteoglycan with heparinoid proteoglycan competitive binding angiogenesis factor, thereby block the combination of angiogenesis factor and its receptor, performance suppresses the effect of endothelial cell growth, suppresses tumor collateral blood vessels and forms.The Pseudobulbus Bletillae (Rhizoma Bletillae) also has antiinflammatory, coagulant blood, antiviral, antitumor in addition, the biologic activity such as antioxidation, and as natural macromolecular material, it has functional slow-release, local anelasticity, nonirritant, has no side effect, aboundresources, the characteristic such as cheap and easy to get.
PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere prepared by the present invention, combine the advantage of PLGA and the Pseudobulbus Bletillae (Rhizoma Bletillae), not only can regulate by adjusting PLGA ratio the degradation speed of microsphere, and contribute to suppress collateral blood vessels formation adding of Pseudobulbus Bletillae polysaccharose, the foster blood supply of effectively cutting off tumor supplies.Along with the degraded of PLGA in microsphere, Pseudobulbus Bletillae (Rhizoma Bletillae) granule wherein can arrive more minute blood vessel, and further occlusion of bone tumors blood vessel, reaches the further therapeutical effect to tumor, and its effect is that single PLGA microsphere or Pseudobulbus Bletillae (Rhizoma Bletillae) microsphere institute is inaccessiable.
summary of the invention
The object of this invention is to provide a kind of thromboembolism PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere and preparation method thereof.
PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism provided by the present invention, described complex microsphere is made up of PLGA and Pseudobulbus Bletillae polysaccharose, microsphere features smooth surface, particle diameter is regular, and the part by weight of PLGA and Pseudobulbus Bletillae polysaccharose is 95:5 ~ 80:20, and particle diameter is 50 ~ 1000 μ m.
The present invention also provides the preparation method of a kind of thromboembolism PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere, and concrete steps are as follows:
(1) PLGA is dissolved in organic solvent, PLGA organic solution and the ultrasonic 8-12min that mixes of Pseudobulbus Bletillae polysaccharose aqueous solution, be dispersed in PLGA organic solution Pseudobulbus Bletillae polysaccharose aqueous solution, obtains emulsion;
(2) in the emulsion obtaining to step (1), add ethylenediamine solution, continue ultrasonic 8-12min, make ethylenediamine and Pseudobulbus Bletillae polysaccharose aqueous solution, to be cross-linked Pseudobulbus Bletillae polysaccharose, obtain Water-In-Oil mixed emulsion;
(3) step (2) gained Water-In-Oil mixed emulsion is added dropwise in the 0.8%PVA aqueous solution under stirring condition, emulsion dispersion forms fine droplet, after 10-14h, organic solvent volatilization, Pseudobulbus Bletillae polysaccharose is crosslinked, and PLGA and the Pseudobulbus Bletillae (Rhizoma Bletillae) are separated out, and forms solidified microsphere, by the washing of products therefrom sucking filtration, lyophilization obtains product.
In the present invention, the purity of Pseudobulbus Bletillae polysaccharose used is greater than 90%, and the concentration of Pseudobulbus Bletillae polysaccharose aqueous solution is 10%.
In the present invention, the ethylenediamine concentration of use is 5% ~ 10%.
In the present invention, the organic solvent that dissolves PLGA is dichloromethane or chloroform.
In the present invention, PLGA organic solution and Pseudobulbus Bletillae polysaccharose aqueous solution volume ratio example are 4:1 ~ 10:1.
In the present invention, the volume of PVA aqueous solution is 3 ~ 10 times of Water-In-Oil mixed emulsion volume.
Compared with prior art, innovation of the present invention is as follows:
The features such as that material therefor PLGA of the present invention and Pseudobulbus Bletillae polysaccharose all have is biodegradable, nontoxic, good biocompatibility.PLGA can adjust its degradation speed by adjusting Acetic acid, hydroxy-, bimol. cyclic ester and lactide ratio and molecular weight as degradation material.Pseudobulbus Bletillae polysaccharose is used widely as Chinese medicine, and its source is abundant, and material is cheap and easy to get.PLGA/ Pseudobulbus Bletillae polysaccharose complex microsphere can be adjusted by adjusting PLGA material the degradation speed of microsphere, thereby be applicable to clinical needs, and adding of Pseudobulbus Bletillae polysaccharose can suppress tumor collateral blood vessels to form, this is that single PLGA or Pseudobulbus Bletillae (Rhizoma Bletillae) embolism materials are not available.Along with the degraded of PLGA, microsphere disintegrates, and the Pseudobulbus Bletillae (Rhizoma Bletillae) is deviate from small particles form, can the thinner one-level tumor vessel of thromboembolism, reach the object of further embolotherapy.In addition, PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere can also be used for the research of drug loading medicament slow release.The method of the invention processing technology is simple, is easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1: the scanning electron microscope close-up view of the PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere of preparing for the embodiment of the present invention 1;
Fig. 2: the scanning electron microscope exterior view of the PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere of preparing for the embodiment of the present invention 1.
The specific embodiment
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for the present invention is described.The implementation condition adopting in embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
embodiment 1:
PLGA is dissolved in in dichloromethane, to obtain concentration be 40% solution, Pseudobulbus Bletillae polysaccharose concentration of aqueous solution is 10%, both get respectively 16ml and 4ml, by both ultrasonic 10min under ultrasonic power 360w, add 10% ethylenediamine solution to continue ultrasonic 10min afterwards in above mixed liquor.In 250ml flask, add 0.8% PVA aqueous solution 100ml, be slowly added dropwise in the mixed liquor of above-mentioned preparation, control mixing speed 300rpm, curing reaction 12h, washes sucking filtration by products obtained therefrom, obtains PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere after lyophilization.
The above-mentioned spherical rounding of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere making, mean diameter is 500 μ m, and PLGA/ Pseudobulbus Bletillae polysaccharose mass ratio is that 95:5(measuring method is: take a certain amount of product and be positioned in dichloromethane solution, dissolve the PLGA in complex microsphere, again that surplus products are dry, the calculating of weighing).
embodiment 2:
PLGA is dissolved in in dichloromethane, to obtain concentration be 10% solution, Pseudobulbus Bletillae polysaccharose concentration of aqueous solution is 10%, and both get respectively 16ml and 4ml, by both ultrasonic 10min under ultrasonic power 270w, in above mixed liquor, add 10% ethylenediamine solution afterwards, continue ultrasonic 10min.In 250ml flask, add 0.8% PVA aqueous solution 100ml, be slowly added dropwise in the mixed liquor of above-mentioned preparation, control mixing speed 500rpm, curing reaction 12h, washes sucking filtration by products obtained therefrom, obtains PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere after lyophilization.
The above-mentioned spherical rounding of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere making, mean diameter is 80 μ m, and PLGA/ Pseudobulbus Bletillae polysaccharose mass ratio is that 80:20(measuring method is: take a certain amount of product and be positioned in dichloromethane solution, dissolve the PLGA in complex microsphere, again that surplus products are dry, the calculating of weighing).
embodiment 3:
PLGA is dissolved in in dichloromethane, to obtain concentration be 20% solution, Pseudobulbus Bletillae polysaccharose concentration of aqueous solution is 10%, and both get respectively 18ml and 2ml, by both ultrasonic 10min under ultrasonic power 360w, to the ethylenediamine solution that adds 10% in above mixed liquor, continue ultrasonic 10min afterwards.In 250ml flask, add 0.8% PVA aqueous solution 100ml, be slowly added dropwise in the mixed liquor of above-mentioned preparation, control mixing speed 400rpm, curing reaction 12h, washes sucking filtration by products obtained therefrom, obtains PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere after lyophilization.
The above-mentioned spherical rounding of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere making, mean diameter is 320 μ m, and PLGA/ Pseudobulbus Bletillae polysaccharose mass ratio is that 95:5(measuring method is: take a certain amount of product and be positioned in dichloromethane solution, dissolve the PLGA in complex microsphere, again that surplus products are dry, the calculating of weighing).
embodiment 4:
PLGA is dissolved in in dichloromethane, to obtain concentration be 10% solution, Pseudobulbus Bletillae polysaccharose concentration of aqueous solution is 8%, and both get respectively 16ml and 4ml, by both ultrasonic 10min under ultrasonic power 360w, to the ethylenediamine solution that adds 10% in above mixed liquor, continue ultrasonic 10min afterwards.In 250ml flask, add 0.8% PVA aqueous solution 100ml, be slowly added dropwise in the mixed liquor of above-mentioned preparation, control mixing speed 400rpm, curing reaction 12h, washes sucking filtration by products obtained therefrom, obtains PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere after lyophilization.
The above-mentioned spherical rounding of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere making, mean diameter is 370 μ m, and PLGA/ Pseudobulbus Bletillae polysaccharose mass ratio is that 84:16(measuring method is: take a certain amount of product and be positioned in dichloromethane solution, dissolve the PLGA in complex microsphere, again that surplus products are dry, the calculating of weighing).
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalent transformations that spirit is done according to the present invention or modification, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. a PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism, is characterized in that: described complex microsphere is made up of PLGA and Pseudobulbus Bletillae polysaccharose, microsphere features smooth surface, and particle diameter is regular, and the part by weight of PLGA and Pseudobulbus Bletillae polysaccharose is 95:5 ~ 80:20, and particle diameter is 50 ~ 1000 μ m.
2. a preparation method for PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism as claimed in claim 1, is characterized in that concrete steps are as follows:
(1) PLGA is dissolved in organic solvent, PLGA organic solution and the ultrasonic 8-12min that mixes of Pseudobulbus Bletillae polysaccharose aqueous solution, be dispersed in PLGA organic solution Pseudobulbus Bletillae polysaccharose aqueous solution, obtains emulsion;
(2) in the emulsion obtaining to step (1), add ethylenediamine solution, continue ultrasonic 8-12min, make ethylenediamine and Pseudobulbus Bletillae polysaccharose aqueous solution, to be cross-linked Pseudobulbus Bletillae polysaccharose, obtain Water-In-Oil mixed emulsion;
(3) step (2) gained Water-In-Oil mixed emulsion is added dropwise in the 0.8%PVA aqueous solution under stirring condition, emulsion dispersion forms fine droplet, after 10-14h, organic solvent volatilization, Pseudobulbus Bletillae polysaccharose is crosslinked, and PLGA and the Pseudobulbus Bletillae (Rhizoma Bletillae) are separated out, and forms solidified microsphere, by the washing of products therefrom sucking filtration, lyophilization obtains product.
3. the preparation method of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism according to claim 2, is characterized in that: the purity of Pseudobulbus Bletillae polysaccharose used is greater than 90%, and the concentration of Pseudobulbus Bletillae polysaccharose aqueous solution is 10%.
4. the preparation method of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism according to claim 2, is characterized in that: the ethylenediamine concentration of use is 5% ~ 10%.
5. the preparation method of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism according to claim 2, is characterized in that: the organic solvent that dissolves PLGA is dichloromethane or chloroform.
6. the preparation method of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism according to claim 2, is characterized in that: PLGA organic solution and Pseudobulbus Bletillae polysaccharose aqueous solution volume ratio are 4:1 ~ 10:1.
7. the preparation method of PLGA/ Pseudobulbus Bletillae (Rhizoma Bletillae) complex microsphere for thromboembolism according to claim 2, is characterized in that: the volume of PVA aqueous solution is 3 ~ 10 times of Water-In-Oil mixed emulsion volume.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108114310A (en) * | 2017-12-22 | 2018-06-05 | 张海军 | A kind of degradable high drug load embolism microball and preparation method thereof |
| CN112043861A (en) * | 2020-09-10 | 2020-12-08 | 穆永旭 | Bletilla striata microsphere for embolism and preparation method thereof |
| CN112043859A (en) * | 2020-09-10 | 2020-12-08 | 穆永旭 | Visual composite microsphere for embolism and preparation method thereof |
| CN114748674A (en) * | 2022-04-18 | 2022-07-15 | 上海方润介入器械有限公司 | Embolism microsphere preloaded with medicine and processing method thereof |
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Patent Citations (3)
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| CN1424111A (en) * | 2002-12-20 | 2003-06-18 | 上海医药工业研究院 | Hyacinth bletilla micro-balls for liver and kidney arterial embolism |
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| US20120121716A1 (en) * | 2007-05-11 | 2012-05-17 | Nerviano Medical Sciences S.R.L. | Pharmaceutical composition of an anthracycline |
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| 陈红宇 等: "中药微球介入治疗肿瘤的研究进展", 《世界华人消化杂志》, vol. 18, no. 22, 8 August 2010 (2010-08-08), pages 2350 - 2354 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108114310A (en) * | 2017-12-22 | 2018-06-05 | 张海军 | A kind of degradable high drug load embolism microball and preparation method thereof |
| CN108114310B (en) * | 2017-12-22 | 2022-11-25 | 张海军 | Degradable drug-loaded microsphere and preparation method thereof |
| CN112043861A (en) * | 2020-09-10 | 2020-12-08 | 穆永旭 | Bletilla striata microsphere for embolism and preparation method thereof |
| CN112043859A (en) * | 2020-09-10 | 2020-12-08 | 穆永旭 | Visual composite microsphere for embolism and preparation method thereof |
| CN114748674A (en) * | 2022-04-18 | 2022-07-15 | 上海方润介入器械有限公司 | Embolism microsphere preloaded with medicine and processing method thereof |
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