CN106110323A - A kind of gold hydroxyl butyl aquagel and its preparation method and application - Google Patents
A kind of gold hydroxyl butyl aquagel and its preparation method and application Download PDFInfo
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- CN106110323A CN106110323A CN201610529522.XA CN201610529522A CN106110323A CN 106110323 A CN106110323 A CN 106110323A CN 201610529522 A CN201610529522 A CN 201610529522A CN 106110323 A CN106110323 A CN 106110323A
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- gold
- hydroxyl butyl
- aquagel
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
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- 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
- A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
Abstract
The invention discloses a kind of gold hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution.The invention also discloses the preparation method of above-mentioned gold hydroxyl butyl aquagel, comprise the steps: to mix gold colloid solution and hydroxyl butyl chitosan aqueous solution, irradiate with laser and obtain gold hydroxyl butyl aquagel.The invention also discloses the application in the medicine of preparation treatment tumor of the above-mentioned gold hydroxyl butyl aquagel.The present invention no longer inspires the change of effect between hydroxyl butyl chitosan molecule by this noncontrollable factors of physiological temp and forms hydrogel, but by the photothermal conversion effect active control hydroxyl butyl chitosan molecule catch cropping of nanometer gold in order to reach fixed point, timing forms the purpose of hydrogel, the lesions position fixed point in regulation is so conducive to form gel, and it is avoided that the injury to normal surrounding tissue, increase the lethality to focus, improve therapeutic effect.
Description
Technical field
The present invention relates to hydroxyl butyl aquagel technical field, particularly relate to a kind of gold-hydroxyl butyl chitosan water-setting
Glue and its preparation method and application.
Background technology
In recent years, at biomedical sector, situ-gel gradually causes the attention of people, and it can provide a kind of simple
Treatment means.Macromolecular solution is by chemical crosslinking, polymerization or change such as pH, temperature etc. by external environment condition, shape in position
Become gel.Wherein, thermo-responsive hydro gel becomes the focus of biomaterial research, and it mainly has the advantage that easy to operate have can
Injectivity, need not in gelation process add other chemical cross-linking agent, without complex operations and then improve in gelation process
The biological safety of material and the compatibility.
Hydroxyl butyl chitosan because of its special temperature sensitive performance, as a kind of novel biomaterial have widely should
Use prospect.The hydroxyl butyl chitosan of the preparation such as Wei can keep liquid in less than the physiological environment of body temperature for a long time, when temperature raises
During to physiological body temperature, in 60s, form hydrogel.Therefore between abdominal wall and caecum wall, the most lasting barrier is formed, prevention
The generation of postoperative peritoneal adhesions.Liu Shuanli etc. have detected the effect in terms of cerebrospinal fluid leakproof of the Thermo-sensitive hydroxyl butyl chitosan.King
The synthetic method improving hydroxyl butyl chitosan such as pretty, is used for Bao Zaikang by the Thermo-sensitive hydroxyl butyl aquagel of preparation
Cancer drug amycin.Test result indicate that through modified hydroxyl butyl chitosan, there is Thermo-sensitive, plastic under physiological temp
Property good, load chemicals can be wrapped, and in drug release process, play certain control action.
Currently, with respect to hydroxyl butyl chitosan in situ formed gel process be all by reaching physiological temp after, cause former
The hydrogen bond action of the cohesion of this obstruction hydroxyl butyl chitosan molecule weakens, and intermolecular is mutually wrapped in because of hydrophobic interaction
Together, hydrogel is ultimately formed.Form gel by physiological temp regulation be applied to a lot of field although this, but due to
Macromolecular solution internal has reached physiological temp once enter, so it is difficult to ensure that formed solidifying at the lesions position of regulation
Glue, and then reduce its usability, during particularly with treating malignant tumor, its practical application effect of strong influence.
In treating malignant tumor means, photo-thermal therapy technology is a kind of novel therapeutic technology, utilizes nanometer photothermal conversion
The luminous energy of the near-infrared laser of absorption is converted into heat energy by agent, kills tumor cell by localized hyperthermia, have quick, efficient,
The advantage such as Wicresoft and low toxicity, shows good application prospect in the treatment of Several Kinds of Malignancy.For improving photo-thermal therapy effect
Really, needing to explore efficient photothermal deformation technology, synthesis different-shape inorganic nano material such as nanometer gold, sheet are attempted in a lot of researchs
Shape palladium, carbon nanomaterial, organic material such as dyestuff, polyaniline, or composite improve photo-thermal conversion efficiency；Also there is research
Concentrate on and utilize coupling antibody to improve cell recognition, increase the photothermal converting agent concentration at tumor locus, improve treatment and imitate
Really.But, the formation that the photothermal conversion characteristic of nanometer gold directly applies to temperature-sensitive hydrogel is rarely had report.
Summary of the invention
The technical problem existed based on background technology, the present invention propose a kind of gold-hydroxyl butyl aquagel and
Preparation method and application, the present invention is no longer inspired by this noncontrollable factors of physiological temp and acts between hydroxyl butyl chitosan molecule
Change form hydrogel, but by the photothermal conversion effect active control hydroxyl butyl chitosan molecule catch cropping of nanometer gold in order to
Reaching fixed point, timing forms the purpose of hydrogel, is so conducive to the lesions position fixed point in regulation to form gel, and is avoided that
Injury to normal surrounding tissue, increases the lethality to focus, improves therapeutic effect.
A kind of gold-hydroxyl butyl aquagel that the present invention proposes, its raw material includes: gold colloid solution and hydroxyl butyl shell
Water solution.
Preferably, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 1-4:8-12.
Preferably, in hydroxyl butyl chitosan aqueous solution, bulking value (g/mL) ratio of hydroxyl butyl chitosan and water is 0.2-
1:10.
Preferably, hydroxyl butyl chitosan aqueous solution need to be prepared under conditions of temperature≤-4 DEG C.
Preferably, in gold colloid solution, the particle diameter of gold is 1-20nm.
Preferably, in gold colloid solution preparation process, aqueous solution of chloraurate is heated to boiling, adds sodium citrate water
Solution and the mixed liquor of polyvinylpyrrolidone, mixing, keep fluidized state >=5min, obtain gold colloid solution.
Preferably, in gold colloid solution preparation process, the concentration of aqueous solution of chloraurate is 0.01-0.02mol/L.
Preferably, in gold colloid solution preparation process, the mass fraction of sodium citrate aqueous solution is 1-2wt%.
Preferably, in gold colloid solution preparation process, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:
1-5。
Preferably, in gold colloid solution preparation process, polyvinylpyrrolidone and gold chloride mass ratio are 0.5-3:1.
The invention allows for the preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprise the steps: gold size
Liquid solution and the mixing of hydroxyl butyl chitosan aqueous solution, irradiate with laser and obtain gold-hydroxyl butyl aquagel.
Preferably, irradiate 20-60s with laser and obtain gold-hydroxyl butyl aquagel.
Preferably, the wavelength of laser is 530-534nm, and power is 150-250mw.
The invention allows for the application in the medicine of preparation treatment tumor of the above-mentioned gold-hydroxyl butyl aquagel.
Above-mentioned water is purified water.
The present invention no longer inspires the change of effect between hydroxyl butyl chitosan molecule by this noncontrollable factors of physiological temp
Form hydrogel, but by the photothermal conversion effect active control hydroxyl butyl chitosan molecule catch cropping of nanometer gold in order to reach fixed
Point, timing form the purpose of hydrogel；By nanometer gold, luminous energy is changed into heat energy under laser irradiates, and then promote Thermo-sensitive
Hydroxyl butyl chitosan forms hydrogel, is evenly coated at by nanometer gold in hydroxyl butyl aquagel and obtains gold-hydroxyl butyl shell
Polysaccharide hydrogel, is so conducive to the lesions position fixed point in regulation to form gel, and hydroxyl butyl aquagel is uniform
Cladding nanometer gold, can avoid the heat that nanometer gold and nanometer gold produce to normal surrounding tissue diffusion, conduction, cause around
The problems such as normal structure excess calories accumulation, it is to avoid the injury to normal surrounding tissue, increase the nanometer gold lethality to focus,
Improve therapeutic effect.
Accompanying drawing explanation
Fig. 1 is turning of gold-hydroxyl butyl aquagel Sol-gel States after laser pre-irradiation of proposing of the present invention
Become figure.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and irradiates with laser and obtains gold-hydroxyl butyl aquagel.
Embodiment 2
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 1:12, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 0.2:10, and in gold colloid solution, the particle diameter of gold is 20nm.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and irradiates 20s with laser and obtains gold-hydroxyl butyl aquagel.
Embodiment 3
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 4:8, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 1:10, and in gold colloid solution, the particle diameter of gold is 1nm；
In gold colloid solution preparation process, it is that 0.02mol/L aqueous solution of chloraurate is heated to boiling by concentration, adds matter
Amount mark is the mixed liquor of 1wt% sodium citrate aqueous solution and polyvinylpyrrolidone, and mixing keeps fluidized state 10min,
To gold colloid solution, wherein, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:5, polyvinylpyrrolidone and chlorine
Auric acid mass ratio is 0.5:1.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and is 534nm with wavelength, and power is that the laser irradiation 60s of 150mw obtains gold-hydroxyl butyl chitosan water
Gel.
Embodiment 4
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 2:11, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 0.4:10, and in gold colloid solution, the particle diameter of gold is 15nm；
In gold colloid solution preparation process, it is that 0.012mol/L aqueous solution of chloraurate is heated to boiling by concentration, adds
Mass fraction is the mixed liquor of 1.8wt% sodium citrate aqueous solution and polyvinylpyrrolidone, mixing, keeps fluidized state
15min, obtains gold colloid solution, and wherein, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:2, polyvinyl pyrrole
Alkanone and gold chloride mass ratio are 2.5:1.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and is 530nm with wavelength, and power is that the laser irradiation 30s of 250mw obtains gold-hydroxyl butyl chitosan water
Gel.
Embodiment 5
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 3:9, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 0.8:10, and in gold colloid solution, the particle diameter of gold is 5nm；
In gold colloid solution preparation process, it is that 0.018mol/L aqueous solution of chloraurate is heated to boiling by concentration, adds
Mass fraction is the mixed liquor of 1.2wt% sodium citrate aqueous solution and polyvinylpyrrolidone, mixing, keeps fluidized state
20min, obtains gold colloid solution, and wherein, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:4, polyvinyl pyrrole
Alkanone and gold chloride mass ratio are 1:1.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and is 533nm with wavelength, and power is that the laser irradiation 40s of 190mw obtains gold-hydroxyl butyl chitosan water
Gel.
Embodiment 6
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 3:10, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 0.5:10, and in gold colloid solution, the particle diameter of gold is 10nm；
In gold colloid solution preparation process, it is that 0.01mol/L aqueous solution of chloraurate is heated to boiling by concentration, adds matter
Amount mark is the mixed liquor of 1wt% sodium citrate aqueous solution and polyvinylpyrrolidone, and mixing keeps fluidized state 5min,
To gold colloid solution, wherein, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:3, polyvinylpyrrolidone and chlorine
Auric acid mass ratio is 1:1.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and is 532nm with wavelength, and power is that the laser irradiation 20s of 200mw obtains gold-hydroxyl butyl chitosan water
Gel.
Observe the preparation process of gold-hydroxyl butyl aquagel in embodiment 6, be that the present invention proposes with reference to Fig. 1, Fig. 1
The transformation figure of gold-hydroxyl butyl aquagel Sol-gel States after laser pre-irradiation.As seen from Figure 1, gold size
Liquid solution is claret after joining hydroxyl butyl chitosan solution, has preferable mobility, and laser forms gel, tool after irradiating
There is certain mechanical strength, be inverted and do not flow.
Embodiment 7
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 1:10, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 1:10, and in gold colloid solution, the particle diameter of gold is 20nm；
In gold colloid solution preparation process, it is that 0.01mol/L aqueous solution of chloraurate is heated to boiling by concentration, adds matter
Amount mark is the mixed liquor of 1wt% sodium citrate aqueous solution and polyvinylpyrrolidone, and mixing keeps fluidized state 6min,
To gold colloid solution, wherein, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:1, polyvinylpyrrolidone and chlorine
Auric acid mass ratio is 3:1.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and is 532nm with wavelength, and power is that the laser irradiation 60s of 200mw obtains gold-hydroxyl butyl chitosan water
Gel.
Embodiment 8
A kind of gold-hydroxyl butyl aquagel, its raw material includes: gold colloid solution and hydroxyl butyl chitosan aqueous solution,
Wherein, the volume ratio of gold colloid solution and hydroxyl butyl chitosan aqueous solution is 1:10, in hydroxyl butyl chitosan aqueous solution, and hydroxyl butyl
Bulking value (g/mL) ratio of chitosan and water is 0.2:10, and in gold colloid solution, the particle diameter of gold is 5nm；
In gold colloid solution preparation process, it is that 0.01mol/L aqueous solution of chloraurate is heated to boiling by concentration, adds matter
Amount mark is the mixed liquor of 1wt% sodium citrate aqueous solution and polyvinylpyrrolidone, and mixing keeps fluidized state 8min,
To gold colloid solution, wherein, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:5, polyvinylpyrrolidone and chlorine
Auric acid mass ratio is 2:1.
The preparation method of above-mentioned gold-hydroxyl butyl aquagel, comprises the steps: gold colloid solution and hydroxyl butyl
Chitosan aqueous solution mixes, and is 532nm with wavelength, and power is that the laser irradiation 40s of 200mw obtains gold-hydroxyl butyl chitosan water
Gel.
Test example 1
Selecting human cervical carcinoma cell is the object of extracorporeal simulating experiment.With embodiment 8 as test group, observe gold-hydroxyl fourth
The effect to HeLa cell of the base aquagel, and with common gold nano medicine as matched group, result is as follows:
Test group: cultivation HeLa cell is to HeLa cell attachment in CO2 gas incubator, is subsequently adding in embodiment 8
Gold colloid solution and hydroxyl butyl chitosan aqueous solution laser irradiate 40s.Can observe at HeLa thin by fluorescence microscope
Cellular surface forms gold-hydroxyl butyl aquagel, and nanometer gold is not distributed in culture fluid.
Matched group: cultivation HeLa cell is to HeLa cell attachment in CO2 gas incubator, is subsequently adding common Jenner
Rice medicine laser irradiate 40s.Although being can observe by fluorescence microscope and being covered with some common Jenners at HeLa cell surface
Rice medicine, but in culture fluid, also random dispersion common gold nano medicine.
By the above results it can be seen that polar group on hydroxyl butyl chitosan in gold-hydroxyl butyl aquagel
Can be with the effect by hydrogen bond of the polysaccharide of HeLa cell surface, protein or phospholipid so that hydroxyl butyl chitosan adheres to
On HeLa cell, pinpoint, be positioned at HeLa cell surface formation gel, and hydroxyl butyl aquagel is uniformly coated with nanometer
Gold, it is to avoid nanometer gold is to outer scattered.
Above-mentioned HeLa cell is derived from the cell of the cervical cancer cell of a Black American women Henrietta Lacks
System.HeLa cell is a kind of artificial culture, has the cell of unlimited multiplication capacity, is widely used in tumor research, biology in fact
Test or cell is cultivated.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (10)
1. gold-hydroxyl butyl aquagel, it is characterised in that its raw material includes: gold colloid solution and hydroxyl butyl shell gather
Sugar aqueous solution.
Gold-hydroxyl butyl aquagel the most according to claim 1, it is characterised in that gold colloid solution and hydroxyl butyl shell
The volume ratio of water solution is 1-4:8-12.
Gold the most according to claim 1 or claim 2-hydroxyl butyl aquagel, it is characterised in that hydroxyl butyl chitosan aqueous solution
In, bulking value (g/mL) ratio of hydroxyl butyl chitosan and water is 0.2-1:10.
4. according to gold described in any one of claim 1-3-hydroxyl butyl aquagel, it is characterised in that hydroxyl butyl chitosan
Aqueous solution need to be prepared under conditions of temperature≤-4 DEG C.
5. according to gold described in any one of claim 1-4-hydroxyl butyl aquagel, it is characterised in that in gold colloid solution
The particle diameter of gold is 1-20nm.
6. according to gold described in any one of claim 1-5-hydroxyl butyl aquagel, it is characterised in that in gold colloid solution
In preparation process, aqueous solution of chloraurate is heated to boiling, adds sodium citrate aqueous solution and the mixing of polyvinylpyrrolidone
Liquid, mixing, keep fluidized state >=5min, obtain gold colloid solution.
Gold-hydroxyl butyl aquagel the most according to claim 6, it is characterised in that in gold colloid solution preparation process
In, the concentration of aqueous solution of chloraurate is 0.01-0.02mol/L；Preferably, in gold colloid solution preparation process, sodium citrate
The mass fraction of aqueous solution is 1-2wt%.
Gold-hydroxyl butyl aquagel the most according to claim 6, it is characterised in that in gold colloid solution preparation process
In, aqueous solution of chloraurate, the volume ratio of sodium citrate aqueous solution are 1:1-5；Preferably, in gold colloid solution preparation process,
Polyvinylpyrrolidone and gold chloride mass ratio are 0.5-3:1.
9. the preparation method of gold as described in any one of claim 1-8-hydroxyl butyl aquagel, it is characterised in that
Comprise the steps: to mix gold colloid solution and hydroxyl butyl chitosan aqueous solution, obtain gold-hydroxyl butyl shell with laser irradiation and gather
Sucrose solution gel；Preferably, irradiate 20-60s with laser and obtain gold-hydroxyl butyl aquagel；Preferably, the wavelength of laser is
530-534nm, power is 150-250mw.
10. gold as described in any one of claim 1-8-hydroxyl butyl aquagel is in the medicine of preparation treatment tumor
Application.
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