CN107583049A - A kind of preparation method of the syringeability hydrogel with light thermal property - Google Patents
A kind of preparation method of the syringeability hydrogel with light thermal property Download PDFInfo
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- CN107583049A CN107583049A CN201710820795.4A CN201710820795A CN107583049A CN 107583049 A CN107583049 A CN 107583049A CN 201710820795 A CN201710820795 A CN 201710820795A CN 107583049 A CN107583049 A CN 107583049A
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Abstract
A kind of preparation method of the syringeability hydrogel with light thermal property, belongs to field of functional materials.The present invention based on the phenomenon that multiple medication treatment is needed in treating malignant tumor, propose it is a kind of by shot medicine and the method repeatedly treated.The sodium alginate large biological molecule (Alg DA) of dopamine modification is prepared for first；Regulate and control chitosan (CS) and the gelling temperature of β sodium glycero-phosphates (β GP) temperature-sensitive hydrogel (CGP) in Human Physiology temperature, make it have reached at normal temperatures for colloidal sol after human body be gel characteristic；The temperature-sensitive hydrogel with syringeability is prepared after Alg DA are mixed with CGP, the gold nanorods (Au PDA NRs) of previously prepared poly-dopamine parcel are adulterated inside it again, obtain the syringeability hydrogel (CGP/Alg DA@Au PDA) with light thermal property.Au NRs can be fixed on tumor locus by the gel, the multiple photothermal deformation under laser irradiation, and the purpose for the treatment of tumour is realized using high temperature.The obtained syringeability hydrogel with light thermal property has potential application value in bio-medical field.
Description
Technical field
A kind of syringeability hydrogel with light thermal property, belongs to technical field of function materials.
Background technology
For in treating malignant tumor, by medicine by body-internal-circulation system transfer to diseased region, being treated so as to reach
Purpose.But non-specific distribution in transportation system's body of medicine, external etc. a series of ask may be removed by quick
Topic.Hydrogel can be fixed on the release medicine of lesions position continuous and effective as a kind of local medicine-applying system, therefore, it is possible to
Load capacity and the residence time of medicine are selected according to the deterioration degree of disease, is effectively solved the above problems.Due to pernicious swollen
The invasion and the resistance to the action of a drug of knurl, need repeatedly to be administered in therapeutic process, not only therapeutic efficiency is limited returns patient and bring
Very big pain.Photo-thermal therapy (PTT) based on nano material is a kind of minimally invasive oncotherapy technology developed rapidly in recent years.
Light thermit powder is after tumor locus accumulation, under the exciting of incident light, makes lesion locations using heat caused by photothermal deformation effect
Temperature raises, and reaches the effect that killing tumor cell is realized after certain temperature.Moreover, can repeatedly be irradiated at same position, reach
The purpose that a shot is repeatedly treated.More photothermal deformation agent is studied at present to receive including gold nano grain, graphene oxide, carbon
Mitron, organic dyestuff etc..Wherein, gold nanorods (Au NRs) have stable chemical property, excellent optical property and good
Biocompatibility, be easy to the advantages that surface modification, be used widely in tumor thermal therapy field.By sensitising agent Au NRs
Fixation is embedded in the hydrogel containing a large amount of pore passage structures, realizes that it stops in the long-time of tumor locus after being injected in vivo
Stay, and then multiple photo-thermal therapy is carried out according to tumor type and deterioration degree.
For make hydrogel can direct injection, the temperature sensitive hydrogel that can respond variation of ambient temperature causes research
The interest of person.Temperature-sensitive gel can change the transformation that sol-gel occurs with temperature.Part thermo-responsive hydro gel material
Gelling temperature is colloidal sol at normal temperatures, has syringeability, but be transformed into after being injected into vivo close to Human Physiology temperature
Gel, therefore such thermo-responsive hydro gel can be used as pharmaceutical carrier, be treated for local injection, there is good answer in bio-medical
Use prospect.Wherein based on the temperature-sensitive hydrogel of chitosan/sodium β-glycerophosphate (CS/ β-GP, CGP) in medicament transport, cell
The fields such as support obtain extensive concern.It is frangible but research shows that the mechanical performance of CGP temperature-sensitive hydrogels is poor, in biology
It is difficult to maintain its intact form in vivo.Lack limit to improve these, researchers by its with other such as hydroxyethyl cellulose, bright
The large biological molecules such as glue, polyvinyl alcohol, sodium alginate are mixed to get compound temperature-sensitive hydrogel, its mechanical strength available one
Fixed enhancing.But it is still without photo-thermal/photodynamic effect, the effect of " shot, repeatedly treatment " can not be met.
The present invention is compound with the sodium alginate of dopamine modification by it using CGP temperature-sensitive hydrogels as primary raw material；Simultaneously
Preparing the modification gold nanorods with suitable draw ratio makes plural gel with photothermal conversion effect, can be according to different tumor types
Suitable treatment time is selected with different deterioration degrees, avoids multiple drug injection and multiple drug cycles normal tissue
Side effect, had broad application prospects in biomedicine fields such as tumor thermal therapies.
The content of the invention
It is contemplated that prepare chitosan/sodium alginate syringeability water-setting that the gold nanorods with light thermal property adulterate
Glue.
Technical scheme：Utilize the solidifying of the temperature-sensitive hydrogel of chitosan (CS) and sodium β-glycerophosphate (β-GP)
Gelatinization temperature can control the characteristic in Human Physiology temperature；By previously prepared dopamine be modified alginic acid (Alg-DA) with
CS, β-GP are mixed with to obtain the temperature-sensitive hydrogel with syringeability (CGP/Alg-DA), and poly- DOPA is adulterated inside it
The gold nanorods (Au-PDA NRs) of amine parcel, utilize the adhesive attraction between the dopamine and Alg-DA on Au NRs surfaces, Au-
PDA NRs uniform and stable can be dispersed in inside gel, obtain the syringeability hydrogel (CGP/ with light thermal property
Alg-DA@Au-PDA)。
Dopamine is by amidation process graft modification sodium alginate, and the mol ratio control of dopamine and sodium alginate is 1:
1~1:5, the grafting rate of dopamine can be controlled in 9%~50%, is expressed as Alg-DA, and its structural formula is as follows.
60 ± 2nm is grown using seed mediated growth method control gold nanorods, wide 16 ± 4nm, draw ratio is about 4.0, and its LSPR is special
Absworption peak is levied at 830nm.By oxidation autohemagglutination characteristic of the dopamine in alkaline environment, it is set to be wrapped up around gold nanorods
Uniform poly-dopamine layer, controls its thickness in 5.0~9.0nm.
Beneficial effects of the present invention：Poly-dopamine layer is wrapped up on gold nanorods surface, utilizes the poly- more of gold nanorods surface
The adhesive attraction between dopamine in bar amine layer and sodium alginate strand, gold nanorods can be by mutual between dopamine
Effect and uniform and stable be dispersed in inside gel.The gelation transition temperature control of CGP temperature-sensitive hydrogels is given birth in human body
Manage near temperature, and there is syringeability, optical-thermal conversion material can be effectively fixed on to lesions position, gel after laser irradiation
Temperature can be increased to 64 ± 2.2 DEG C；After repeatedly irradiation, gelling temp can repeatedly raise temperature to 60 ± 2.5 DEG C；Thus can root
The time of photo-thermal therapy is selected according to the type and deterioration degree of tumour.
Brief description of the drawings
Fig. 1 Alg-DA nmr spectrum
Fig. 2 (a) Au NRs, (b) Au-PDA NRs transmission electron microscope picture
Fig. 3 CGP/Alg-DA@Au-PDA temperature-sensitive composite hydrogels irradiate (808nm, 1.50W/cm in laser2) after 10 times
Temperature variation
Embodiment
The preparation of embodiment 1, dopamine graft modification sodium alginate (Alg-DA)
Sodium alginate (2g) is dissolved in 100mL PBS cushioning liquid (0.2mol/L, pH=5.5), until completely dissolved
EDC (3.88g) and NHS (4.68g) are sequentially added, 45min is stirred at normal temperatures, afterwards according to 1:1 mol ratio adds 1.9g
Dopamine hydrochloride (DAHCl), lead to nitrogen with biexhaust pipe, vacuumize, repeatedly for three times, drain the air in flask to prevent
DA is aoxidized.Stirring reaction 24h under normal temperature, after reaction terminates, Light brown solid is obtained with a large amount of ethanol precipitations, then washed with ethanol
Centrifugation three times, will be precipitated and dissolved in deionized water, dialyse three days, freeze-drying, obtain dopamine graft modification sodium alginate, mark
It is designated as Alg-DA1。
It should be noted that the addition of the Dopamine hydrochloride (DA) in embodiment 1 is changed into 5.8g and 9.6g (i.e.
nAlg/nDARespectively 1:3 and 1:5) Alg-DA of different degree of substitution, can be obtained, is calculated separately as Alg-DA3And Alg-DA5。
The preparation for the gold nanorods (Au-PDA NRs) that embodiment 2, poly-dopamine are wrapped up
The preparation of gold nanorods：HAuCl4·3H2O (0.25mL, 0.01mol/L) is added to CTAB (9.75mL, 0.1mol/
L) in solution, slowly stir, then the NaBH by freshly prepared frost storage4Solution (0.6mL, 0.01mol/L) rapidly joins
Into mixed solution, stirring reaction 2min, at least 2h is placed at normal temperatures, obtains seed solution.By HAuCl4·3H2O
(0.5mL, 0.01mol/L), Ag NO3(0.1mL, 0.01mol/L) is well mixed with CTAB (10mL, 0.1mol/L), adds anti-
Bad hematic acid (0.08mL, 0.1mol/L), solution colour is become colorless by yellow.0.2mL HCl (1.0mol/L) are added afterwards to adjust
The pH of section system to 1~2,0.024mL seed solutions are eventually adding, mix slowly 10s, place at least 6h at room temperature, use is ultrapure
Three times, obtained gold nanorods (Au NRs) solution concentration is 0.2nmol/L to water centrifuge washing.
Poly ethyldiol modified gold nanorods (Au-PEG NRs)：The Au NRs solution that 10mL is prepared 7200r/min from
Heart 10min, lower sediment thing is dispersed to 5mL SH-PEG-CH3In the aqueous solution of (2mg/mL, Mw=2000), ultrasonic vibration
3min makes Au NRs fully dispersed, and 16h is then stirred at room temperature, and, obtains Au-PEG NRs with ultra-pure water centrifuge washing three times
Solution.
Poly-dopamine parcel Au-PEG NRs (Au-PDA NRs)：Dopamine-the Tris-HCl for preparing dopamine concentration delays
Solution (0.1mg/mL, pH=8.5) is rushed, 5mL dopamines will be dispersed to after the Au-PEG NRs solution centrifugals of above-mentioned preparation
In Tris-HCl cushioning liquid, ultrasonic vibration 3min, then stirring reaction 30min makes dopamine autohemagglutination be wrapped in Au- at room temperature
PEG NRs surface.Poly-dopamine parcel Au-PEG NRs solution centrifugals wash 3 times, can obtain Au-PDA0.1NRs。
It should be noted that make dopamine-Tris-HCl cushioning liquid in embodiment 2 into 0.25mg/mL and 0.5mg/
ML, the Au-PEG NRs of different poly-dopamine Jacket thickness are can obtain, are designated as Au-PDA respectively0.25NRs and Au-PDA0.5NRs。
Embodiment 3, chitosan/dopamine modified sodium alginate temperature-sensitive hydrogel (CGP/Alg- of gold nanorods doping
DA@Au-PDA) preparation
Gold nanorods (the Au-PDA that the above-mentioned poly-dopamine prepared is wrapped up0.25NRs it is directly scattered) after centrifuge washing
Into Alg-DA solution, ultrasonic 3min, compound gold nanorods is uniformly dispersed in Alg-DA solution, be counted as Alg-
DA@Au-PDA0.25.3mL CS solution is accurately pipetted again, at 4 DEG C, adds 0.5mL β-GP solution, after stirring, is added
A certain amount of Alg-DA@Au-PDA0.25Solution, stirring reaction 30min in ice-water bath.It is placed in 37 DEG C of water bath with thermostatic control, mixes
Solution forms the plural gel of crosslinking, and record forms the time of gel, and the gel of formation is counted as CGP/Alg-DA@Au-PDA0.25
Plural gel.
Claims (8)
- A kind of 1. preparation method of the syringeability hydrogel with light thermal property, it is characterized in that the alginic acid that dopamine is modified Sodium and chitosan, sodium β-glycerophosphate are compound；And then the gold nanorods of poly-dopamine parcel are adulterated inside gel, utilize DOPA Interaction between amine makes gold nanorods uniform and that stablizes is dispersed in inside gel, and noting with light thermal property is prepared Penetrating property temperature-sensitive hydrogel.
- 2. preparation method according to claim 1, it is characterized in that in dopamine graft modification sodium alginate sodium alginate with The mol ratio of dopamine is 1:1~1:5, the grafting rate of dopamine can be controlled in 9%~50%, dopamine modified sodium alginate Structural formula is：It is represented by Alg-DA.
- 3. preparation method according to claim 1, it is characterized in that Alg-DA coagulates with chitosan, the compound of sodium β-glycerophosphate In glue, regulate and control the mass ratio 1 of chitosan and sodium β-glycerophosphate first:5~1:10, make chitosan and sodium β-glycerophosphate gel Gelation transition temperature control at about 37 DEG C；Then according to chitosan and Alg-DA mass ratio 10:0~5:5, add different The Alg-DA of quality, making plural gel, within 30min, the plural gel is expressed as CGP/ for gelation time control at 37 DEG C Alg-DA。
- 4. the preparation method of the gold nanorods of poly-dopamine parcel according to claim 1, it is characterized in that preparing absorption first Peak is expressed as Au NRs in 830nm gold nanorods；Au NRs are modified by mercapto-polyglycol again, existed with improving Au NRs Dispersion stabilization and biocompatibility in water；Finally Au NRs are placed in the alkaline buffer of dopamine, existed using dopamine Self-polymeric reaction in alkaline environment, poly-dopamine is deposited into Au NRs surfaces, obtain the gold nanorods of poly-dopamine parcel, table It is shown as Au-PDA NRs.
- 5. preparation method according to claim 4, it is characterized in that the concentration control of the alkaline buffer solution of dopamine is existed 0.1~0.5mg/mL, its pH are 8.5, and the thickness that poly-dopamine deposits to Au NRs surfaces can be controlled in 5.0~9.0nm.
- 6. preparation method according to claim 1, it is characterized in that by Au-PDA NRs solution that concentration is 0.4nmol/L with The syringeability hydrogel with light thermal property is prepared in above-mentioned CGP/Alg-DA mixing and dopings, and the hydrogel is expressed as CGP/ Alg-DA@Au-PDA。
- 7. preparation method according to claim 6, dopamine and the phase between dopamine in Alg-DA on gold nanorods surface Interaction, Au-PDA NRs can be made to may be homogenously dispersed in gel.
- 8. preparation method according to claim 1, the syringeability hydrogel that the present invention is prepared can consolidate Au NRs Tumor locus is scheduled on, and there is photothermal deformation ability；Upon laser irradiation, temperature can be increased to 64 ± 2.2 DEG C to the gel；Through more After secondary irradiation, gelling temp can repeatedly raise temperature to 60 ± 2.5 DEG C, and the mesh of " shot, multiple photo-thermal therapy " can be achieved 's.
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| CN109260509A (en) * | 2018-11-27 | 2019-01-25 | 浙江海洋大学 | A kind of self assembly contact-type anti-bacterial hydrogel dressing and preparation method thereof based on poly-dopamine and chitosan oligosaccharide |
| CN109705369A (en) * | 2018-12-27 | 2019-05-03 | 暨南大学 | A kind of sodium alginate-dopamine/polyvinyl alcohol hydrogel and the preparation method and application thereof |
| CN110241635A (en) * | 2019-06-17 | 2019-09-17 | 浙江海印数码科技有限公司 | A kind of preparation method of the digit printing viscose fabric modified based on dopamine and acrylate pressure-sensitive adhesive |
| CN110358114A (en) * | 2019-06-12 | 2019-10-22 | 南京信息职业技术学院 | Preparation method of porous silicon/gold nanoparticle composite hydrogel and prepared hydrogel |
| CN110498607A (en) * | 2019-08-21 | 2019-11-26 | 中国科学院上海硅酸盐研究所 | A kind of bioactivity powder and its preparation method and application that multi-functional calcium is silicon base lanthanon adulterated |
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| CN113512208A (en) * | 2021-08-04 | 2021-10-19 | 哈尔滨工业大学 | Preparation method of sodium alginate-based photothermal distillation hydrogel |
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| CN109705369A (en) * | 2018-12-27 | 2019-05-03 | 暨南大学 | A kind of sodium alginate-dopamine/polyvinyl alcohol hydrogel and the preparation method and application thereof |
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