CN105396179A - Medicine-carrying aquogel coating and preparation method and application thereof - Google Patents
Medicine-carrying aquogel coating and preparation method and application thereof Download PDFInfo
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- CN105396179A CN105396179A CN201510822796.3A CN201510822796A CN105396179A CN 105396179 A CN105396179 A CN 105396179A CN 201510822796 A CN201510822796 A CN 201510822796A CN 105396179 A CN105396179 A CN 105396179A
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Abstract
The invention provides a medicine-carrying aquogel coating and a preparation method and application thereof. Alumina aquogel serves as a coating substrate and carries anti-infection medicine, and the nanometer medicine-carrying aquogel coating is obtained; due to the characteristics that alumina aquogel is not degraded and is slowly absorbed by human bodies, the anti-infection medicine carried by the medicine-carrying coating can be stored in the coating all the time, and the anti-infection effect of the coating can be achieved continuously; when the coating is applied to an implant material, a composite implant body is obtained and implanted into a human body, and chronic infection especially the chronic infection caused by the implant material can be effectively stopped when damaged parts are repaired.
Description
Technical field
The invention belongs to hydrogel preparation field, relate to a kind of medicine carrying hydrogel coating and its preparation method and application.
Background technology
Medically often utilize embedded material to repair damaged tissue now, but will prevent the generation that tissue site infects when carrying out tissue repair, the fungistatic effect of tissue renovation material conventional is at present unsatisfactory, usually causes tardus infection.Focus is become for the research can carrying out the medical material of tissue repair.
The multicomponent system that hydrogel consists of three-dimensional crosslinked network structure and medium jointly materials such as polymer, because of its stable in properties, can respond fast the minor variations of environment, cause the concern of many researcheres as novel bio-medical material.The bio-compatible performance utilizing it good, hydrogel can be used for controlled release drug delivery system, immobilized enzyme, artificial organ etc. field.Nano oxidized aluminum matrix is very early by the auxiliary reagent of FDA approval as vaccine, because aluminium oxide is when contacting with blood, body fluid and tissue liquid phase, all show good biocompatibility, do not affect metabolic process, simultaneously can also good carrying active substance, the dispersibility of active substance and biological activity thereof in maintenance vaccine.
Therefore, in view of the various advantages of hydrogel and nano aluminium oxide, expect to utilize it to develop the implantable material of a kind of long-acting bacteriostatic, the problem such as recurrent delayed infection when solving tissue repair.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of medicine carrying hydrogel coating and its preparation method and application.
For reaching this object, the present invention by the following technical solutions:
On the one hand, the invention provides a kind of medicine carrying hydrogel coating, described medicine carrying hydrogel coating take alumina hydrogel as coating matrix, carrying anti-infectives.
Medicine carrying hydrogel coating of the present invention utilizes alumina hydrogel to carry anti-infectives as substrate, due to alumina hydrogel contact with tissue liquid phase time, there is good biocompatibility, do not affect metabolic process, and alumina hydrogel self is not degraded, and human body is very slow to the absorption of alumina hydrogel, therefore this coating can be medicament-carried steadily in the long term, make medicine play persistency effect, play the effect of long-acting bacteriostatic, effectively can prevent the generation of delayed infection.
In the present invention, described coating matrix refers to the matrix material forming medicine carrying hydrogel coating, and it is the main component of medicine carrying hydrogel coating.
In medicine carrying hydrogel coating of the present invention, the amount of the anti-infectives of described alumina hydrogel carrying is the 2-15% of alumina hydrogel quality, such as 2.5%, 3%, 3.5%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 14.5%.
Preferably, in described alumina hydrogel, the mass percentage content of aluminum is 1-3%, such as 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, 2.2%, 2.5%, 2.7%, 2.9% or 3%.
In medicine carrying hydrogel coating of the present invention, described anti-infectives is selected from the combination of any one or at least two kinds in penicillin, cephalosporin, gentamycin, tetracycline, erythromycin, vancomycin, metronidazole, tinidazole, ciprofloxacin, levofloxacin.
Preferably, described anti-infectives is the combination of any one or at least two kinds in nanometer silver, Nano-Zinc or chlorhexidine acetate.
In the present invention, when using two or more drug regimen, the interaction between medicine and medicine should be noted, as long as the medicine of combination does not produce can apply the disadvantageous effect of human body.
In the present invention, the thickness of described medicine carrying hydrogel coating is 100-200nm, such as 100nm, 110nm, 120nm, 130nm, 140nm, 150nm, 160nm, 170nm, 180nm, 190nm or 200nm.
On the other hand, the invention provides the preparation method of medicine carrying hydrogel coating as described in relation to the first aspect, said method comprising the steps of:
(1) with aluminum isopropylate. (Al (C
3h
7o)
3) prepare alumina hydrogel for raw material;
(2) mixed homogeneously with anti-infectives solution by the alumina hydrogel that step (1) obtains, be then coated on substrate by mixed solution, drying obtains described medicine carrying hydrogel coating.
In the present invention, step (1) is described, and to take aluminum isopropylate. as the method that alumina hydrogel prepared by raw material be:
Aluminum isopropylate. is added in deionized water, 10-30min (such as 12min, 15min, 18min, 20min, 23min, 25min, 27min or 29min) is stirred under 60-80 DEG C (such as 62 DEG C, 65 DEG C, 67 DEG C, 69 DEG C, 70 DEG C, 73 DEG C, 75 DEG C, 77 DEG C or 79 DEG C), obtain dispersion liquid, by dispersion liquid supersound process 1-3h (such as 1.1h, 1.3h, 1.5h, 1.7h, 2h, 2.2h, 2.5h, 2.7h or 2.9h), be cooled to room temperature, obtain described alumina hydrogel.
Preferably, in the preparation of alumina hydrogel, relative to 1g aluminum isopropylate., the volume of the deionized water added is 10-30mL, such as 12mL, 15mL, 17mL, 19mL, 20mL, 22mL, 24mL, 26mL, 28mL or 29mL.
In the present invention, aluminum isopropylate. joins in deionized water and can decompose, generate boehmite (AlO (OH)), in this process, the by-product 2-propanol generated can volatilize gradually, then by dispersion liquid in ultrasonic lower process, form boehmite hydrogel, after cooling, obtain aluminium oxide (Al
2o
3h
2o) hydrogel.In gained alumina hydrogel, the mass percentage content of aluminum is 1-3%, such as 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, 2.2%, 2.5%, 2.7%, 2.9% or 3%.
In the preparation process in accordance with the present invention, the described anti-infectives solution of step (2) is anti-infectives is dissolved in the drug solution obtained in buffer or glycerine water solution.
Preferably, described buffer is Tris-hydrochloride buffer or the PBS buffer of pH=7.4.
Preferably, in described glycerine water solution, the mass body volume concentrations of glycerol is 0.2-5%, such as 0.2%, 0.3%, 0.5%, 0.7%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 3.8%, 4%, 4.3%, 4.5%, 4.8% or 5%.
Preferably, relative to 10mg anti-infectives, the volume of buffer used or glycerine water solution is 1-3mL, such as 1.1mL, 1.3mL, 1.5mL, 1.7mL, 1.9mL, 2mL, 2.2mL, 2.4mL, 2.6mL, 2.8mL or 2.9mL.
Preferably, in step (2), relative to 100 μ L alumina hydrogels, the volume of anti-infectives solution used is 30-80 μ L, such as 30 μ L, 33 μ L, 35 μ L, 38 μ L, 40 μ L, 45 μ L, 50 μ L, 55 μ L, 60 μ L, 65 μ L, 68 μ L, 70 μ L, 73 μ L, 75 μ L or 78 μ L.
Preferably, step (2) described substrate is any one in microscope slide, corrosion resistant plate or physics and chemistry plate.In the present invention particular restriction be there is no for described substrate, except the above-mentioned several substrates listed, other levelness can also be used dull and stereotyped preferably.
Preferably, step (2) described coating be utilize Meyer rod repeatedly extrusion until coating evenly.Generally repeatedly to ensure solution coating evenly by extrusion more than three times.
Preferably, step (2) described drying drying at room temperature 1-3h in vacuum drying oven, such as 1.1h, 1.3h, 1.5h, 1.7h, 2h, 2.2h, 2.5h, 2.7h or 2.9h.
As the preferred technical solution of the present invention, the preparation method of medicine carrying hydrogel coating of the present invention specifically comprises the following steps:
(1) add in deionized water by aluminum isopropylate., relative to 1g aluminum isopropylate., the volume of the deionized water added is 10-30mL, stir white precipitate 10-30min at 60-80 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 1-3h, be cooled to room temperature, obtain alumina hydrogel;
(2) anti-infectives is dissolved in buffer or glycerine water solution obtains anti-infectives solution, relative to 10mg anti-infectives, the volume of buffer used or glycerine water solution is 1-3mL, the alumina hydrogel that step (1) obtains is mixed homogeneously with anti-infectives solution, relative to 100 μ L alumina hydrogels, the volume of anti-infectives solution used is 30-80 μ L, then mixed solution is coated on substrate, drying at room temperature 1-3h in vacuum drying oven, obtains described medicine carrying hydrogel coating.
On the other hand, the invention provides a kind of compound implant, it is characterized in that, described compound implant is made up of embedded material and the medicine carrying hydrogel coating being as described in relation to the first aspect coated in embedded material top layer.
Embedded material of the present invention be selected from bone implant material, oral cavity embedded material, joint embedded material or Vascular implantation material any one.
In the present invention, by the following method medicine carrying hydrogel coating can be coated in embedded material top layer: embedded material is placed in surface plate, slowly evenly implantation material surface is dropped in the medicine carrying hydrogel solution (being obtained by mixing by alumina hydrogel and anti-infectives solution) of 200 μ L, rotate curtain coating, this gel evenly curtain coating can be distributed in embedded material top layer, drying at room temperature 1-3h (such as 1.1h in vacuum drying oven, 1.3h, 1.5h, 1.7h, 2h, 2.2h, 2.5h, 2.7h or 2.9h), thus form medicine carrying hydrogel coating on embedded material top layer, obtain compound implant of the present invention.
Compound implant of the present invention can implant, and effectively can stop delayed infection while the reparation to damage location, especially because of the delayed infection that embedded material causes.
On the other hand, the medicine carrying hydrogel coating that the invention provides as described in relation to the first aspect is preparing the application in infection material.
Relative to prior art, the present invention has following beneficial effect:
The present invention is by utilizing alumina hydrogel as coating matrix, carrying anti-infectives, obtain nano drug-carrying hydrogel coating, due to the feature that alumina hydrogel is not degraded and absorption of human body is slow, the anti-infectives that this drug-carried coat can be made to carry is present in coating always, can continue to play its anti-infection effect, when this coatings applications is obtained compound implant in embedded material, this implant is implanted, effectively delayed infection can be being stoped, especially because of the delayed infection that embedded material causes while the reparation to damage location.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below by detailed description of the invention.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
In the present embodiment, prepare medicine carrying hydrogel coating by the following method, specifically comprise the following steps:
(1) 2.5g aluminum isopropylate. is added in 50mL deionized water, stir white precipitate 15min at 80 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 2h, be cooled to room temperature, obtain alumina hydrogel (Al
2o
3h
2o), wherein the mass content of aluminum is 2%.
(2) 10mg anti-infectives penicillin is dissolved in the Tris-hydrochloride buffer (concentration 0.05M) of 1mLpH=7.4 and obtains anti-infectives solution, the alumina hydrogel 100 μ L steps (1) obtained is mixed homogeneously in 1.5mL glass tubing with 50 μ L anti-infectives solution, liquid-transfering gun is then utilized to get 50 μ L mixed solutions on microscope slide (2cm × 2cm size), extrusion 5 coatings are even repeatedly to utilize Meyer rod, be put in drying at room temperature 2h in vacuum drying oven afterwards, obtain medicine carrying hydrogel coating, this coating layer thickness is 100-200nm.
Embodiment 2
In the present embodiment, prepare medicine carrying hydrogel coating by the following method, specifically comprise the following steps:
(1) 2.5g aluminum isopropylate. is added in 25mL deionized water, stir white precipitate 30min at 80 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 1h, be cooled to room temperature, obtain alumina hydrogel (Al
2o
3h
2o), wherein the mass content of aluminum is 3%.
(2) 10mg anti-infectives erythromycin is dissolved in the Tris-hydrochloride buffer (concentration 0.05M) of 2mLpH=7.4 and obtains anti-infectives solution, the alumina hydrogel 100 μ L steps (1) obtained is mixed homogeneously in 1.5mL glass tubing with 80 μ L anti-infectives solution, liquid-transfering gun is then utilized to get 50 μ L mixed solutions on microscope slide (2cm × 2cm size), extrusion 7 coatings are even repeatedly to utilize Meyer rod, be put in drying at room temperature 2h in vacuum drying oven afterwards, obtain medicine carrying hydrogel coating, this coating layer thickness is 150-200nm.
Embodiment 3
In the present embodiment, prepare medicine carrying hydrogel coating by the following method, specifically comprise the following steps:
(1) 2.5g aluminum isopropylate. is added in 75mL deionized water, stir white precipitate 20min at 80 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 3h, be cooled to room temperature, obtain alumina hydrogel (Al
2o
3h
2o), wherein the mass content of aluminum is 1%.
(2) 10mg anti-infectives levofloxacin is dissolved in the Tris-hydrochloride buffer (concentration 0.05M) of 3mLpH=7.4 and obtains anti-infectives solution, the alumina hydrogel 100 μ L steps (1) obtained is mixed homogeneously in 1.5mL glass tubing with 30 μ L anti-infectives solution, liquid-transfering gun is then utilized to get 50 μ L mixed solutions on microscope slide (2cm × 2cm size), extrusion 3 coatings are even repeatedly to utilize Meyer rod, be put in drying at room temperature 1h in vacuum drying oven afterwards, obtain medicine carrying hydrogel coating, this coating layer thickness is 120-180nm.
Embodiment 4
In the present embodiment, prepare medicine carrying hydrogel coating by the following method, specifically comprise the following steps:
(1) 2.5g aluminum isopropylate. is added in 50mL deionized water, stir white precipitate 10min at 60 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 2h, be cooled to room temperature, obtain alumina hydrogel (Al
2o
3h
2o), wherein the mass content of aluminum is 2%.
(2) 10mg anti-infectives nanometer silver is dissolved in the Tris-hydrochloride buffer (concentration 0.05M) of 2mLpH=7.4 and obtains anti-infectives solution, the alumina hydrogel 100 μ L steps (1) obtained is mixed homogeneously in 1.5mL glass tubing with 50 μ L anti-infectives solution, liquid-transfering gun is then utilized to get 50 μ L mixed solutions on microscope slide (2cm × 2cm size), extrusion 3 coatings are even repeatedly to utilize Meyer rod, be put in drying at room temperature 3h in vacuum drying oven afterwards, obtain medicine carrying hydrogel coating, this coating layer thickness is 100-180nm.
Embodiment 5
In the present embodiment, prepare medicine carrying hydrogel coating by the following method, specifically comprise the following steps:
(1) 2.5g aluminum isopropylate. is added in 50mL deionized water, stir white precipitate 15min at 70 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 2h, be cooled to room temperature, obtain alumina hydrogel (Al
2o
3h
2o), wherein the mass content of aluminum is 2%.
(2) 10mg anti-infectives chlorhexidine acetate is dissolved in the Tris-hydrochloride buffer (concentration 0.05M) of 2mLpH=7.4 and obtains anti-infectives solution, the alumina hydrogel 100 μ L steps (1) obtained is mixed homogeneously in 1.5mL glass tubing with 50 μ L anti-infectives solution, liquid-transfering gun is then utilized to get 50 μ L mixed solutions on microscope slide (2cm × 2cm size), extrusion 5 coatings are even repeatedly to utilize Meyer rod, be put in drying at room temperature 2h in vacuum drying oven afterwards, obtain medicine carrying hydrogel coating, this coating layer thickness is 100-200nm.
The bacteriostasis rate of medicine carrying hydrogel coating prepared by embodiment 1-5 is investigated, the bacteriostasis rate that the medicine carrying hydrogel coating that table 1 shows embodiment 1-5 continues to the 7th day.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Bacteriostasis rate | 99.4％ | 99.5％ | 99.8％ | ≥99.99％ | ≥99.99％ |
As can be seen from Table 1, the bacteriostasis rate of medicine carrying hydrogel coating of the present invention can reach more than 99%, even reaches more than 99.99%, has good fungistatic effect.
Medicine carrying hydrogel coating the present invention prepared is applied to embedded material, is implanted, and effectively can stop delayed infection while repairing damage location, especially because of the delayed infection that embedded material causes.
Applicant states, the present invention illustrates medicine carrying hydrogel coating of the present invention and its preparation method and application by above-described embodiment, but the present invention is not limited to above-described embodiment, does not namely mean that the present invention must rely on above-described embodiment and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a medicine carrying hydrogel coating, is characterized in that, described medicine carrying hydrogel coating take alumina hydrogel as coating matrix, carrying anti-infectives.
2. medicine carrying hydrogel coating according to claim 1, is characterized in that, the amount of the anti-infectives of described alumina hydrogel carrying is the 2-15% of alumina hydrogel quality.
Preferably, in described alumina hydrogel, the mass percentage content of aluminum is 1-3%.
3. medicine carrying hydrogel coating according to claim 1 and 2, it is characterized in that, described anti-infectives is selected from the combination of any one or at least two kinds in penicillin, cephalosporin, gentamycin, tetracycline, erythromycin, vancomycin, metronidazole, tinidazole, ciprofloxacin, levofloxacin;
Preferably, described anti-infectives is the combination of any one or at least two kinds in nanometer silver, Nano-Zinc or chlorhexidine acetate.
4. the medicine carrying hydrogel coating according to any one of claim 1-3, is characterized in that, the thickness of described medicine carrying hydrogel coating is 100-200nm.
5. the preparation method of the medicine carrying hydrogel coating according to any one of claim 1-4, is characterized in that, said method comprising the steps of:
(1) be that alumina hydrogel prepared by raw material with aluminum isopropylate.;
(2) mixed homogeneously with anti-infectives solution by the alumina hydrogel that step (1) obtains, be then coated on substrate by mixed solution, drying obtains described medicine carrying hydrogel coating.
6. preparation method according to claim 5, is characterized in that, step (1) is described, and to take aluminum isopropylate. as the method that alumina hydrogel prepared by raw material be:
Aluminum isopropylate. is added in deionized water, stir 10-30min at 60-80 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 1-3h, be cooled to room temperature, obtain described alumina hydrogel;
Preferably, relative to 1g aluminum isopropylate., the volume of the deionized water added is 10-30mL.
7. the preparation method according to claim 5 or 6, is characterized in that, the described anti-infectives solution of step (2) is anti-infectives is dissolved in the drug solution obtained in buffer or glycerine water solution;
Preferably, described buffer is Tris-hydrochloride buffer or the PBS buffer of pH=7.4;
Preferably, in described glycerine water solution, the mass body volume concentrations of glycerol is 0.2-5%;
Preferably, relative to 10mg anti-infectives, the volume of buffer used or glycerine water solution is 1-3mL;
Preferably, in step (2), relative to 100 μ L alumina hydrogels, the volume of anti-infectives solution used is 30-80 μ L;
Preferably, step (2) described substrate is any one in microscope slide, corrosion resistant plate or physics and chemistry plate;
Preferably, step (2) described coating be utilize Meyer rod repeatedly extrusion until coating evenly;
Preferably, step (2) described drying drying at room temperature 1-3h in vacuum drying oven.
8. the preparation method according to any one of claim 5-7, is characterized in that, said method comprising the steps of:
(1) add in deionized water by aluminum isopropylate., relative to 1g aluminum isopropylate., the volume of the deionized water added is 10-30mL, stir 10-30min at 60-80 DEG C, obtain dispersion liquid, by dispersion liquid supersound process 1-3h, be cooled to room temperature, obtain alumina hydrogel;
(2) anti-infectives is dissolved in buffer or glycerine water solution obtains anti-infectives solution, relative to 10mg anti-infectives, the volume of buffer used or glycerine water solution is 1-3mL, the alumina hydrogel that step (1) obtains is mixed homogeneously with anti-infectives solution, relative to 100 μ L alumina hydrogels, the volume of anti-infectives solution used is 30-80 μ L, then mixed solution is coated on substrate, drying at room temperature 1-3h in vacuum drying oven, obtains described medicine carrying hydrogel coating.
9. a compound implant, is characterized in that, described compound implant is made up of embedded material and the medicine carrying hydrogel coating according to any one of claim 1-5 being coated in embedded material top layer;
Preferably, described embedded material is selected from any one in bone implant material, oral cavity embedded material, joint embedded material or Vascular implantation material.
10. the medicine carrying hydrogel coating according to any one of claim 1-5 is preparing the application in infection material.
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| WO2003105918A1 (en) * | 2002-06-18 | 2003-12-24 | Surmodics, Inc. | Bioactive agent release coating with aromatic poly(meth)acrylates |
| WO2007140262A2 (en) * | 2006-05-24 | 2007-12-06 | Nellix, Inc. | Material for creating multi-layered films and methods for making the same |
| CN101249285A (en) * | 2007-02-21 | 2008-08-27 | 科迪斯公司 | A coating for a medical device having an anti-thrombotic conjugate |
| CN101264345A (en) * | 2007-11-27 | 2008-09-17 | 天津百畅医疗器械科技有限公司 | Degradable blood vessel stent drug-eluting capable of reducing incidence rate of advanced thrombus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003105918A1 (en) * | 2002-06-18 | 2003-12-24 | Surmodics, Inc. | Bioactive agent release coating with aromatic poly(meth)acrylates |
| WO2007140262A2 (en) * | 2006-05-24 | 2007-12-06 | Nellix, Inc. | Material for creating multi-layered films and methods for making the same |
| CN101249285A (en) * | 2007-02-21 | 2008-08-27 | 科迪斯公司 | A coating for a medical device having an anti-thrombotic conjugate |
| CN101264345A (en) * | 2007-11-27 | 2008-09-17 | 天津百畅医疗器械科技有限公司 | Degradable blood vessel stent drug-eluting capable of reducing incidence rate of advanced thrombus |
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