CN103816841B - A kind of preparation method with the hydrogel of plasma chirality - Google Patents
A kind of preparation method with the hydrogel of plasma chirality Download PDFInfo
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Abstract
There is a preparation method for the hydrogel of plasma chirality, belong to technical field of material chemistry.First the present invention prepares the nanogold particle AuNP-MUA-PEI of modification; then in the AuNP-MUA-PEI aqueous solution, add L-type glutamic acid Fmoc-L-Glu and the L-type lysine L-Lys of the 9-fluorenylmethyloxycarbonyl protection of equimolar amounts; the concentration of control AuNP-MUA-PEI is 1-5nmol/L; the concentration of Fmoc-L-Glu and L-Lys is respectively 0.1-1mol/L; heating makes it dissolve; to be cooled after room temperature, namely define the hydrogel with plasma chirality.The present invention is on the basis of existing hydrogel, introduces noble metal nanometer material, obtains the hydrogel with plasma chirality by self assembly.
Description
Technical field
The present invention relates to a kind of preparation method with the hydrogel of plasma chirality, belong to technical field of material chemistry.
Background technology
Hydrogel take water as a class soft material of decentralized medium, because the physicochemical property of its uniqueness, extensively studied in recent decades by people.Micro-molecular hydrogel is obtained by the non-covalent bond effect self assembly of gelator in aqueous phase, and high-molecular gel be by macromolecular chain between chemical bond or the swelling body of three-dimensional crosslinking structure that formed of physical force, be the compound system formed by solvent and macromolecule network.In recent years, (temperature, pH, pressure, light etc.) can be stimulated to external world to produce the progress in Intelligent Hydrogel of sensitive response change by wide coverage, and it has obtained deep application in fields such as biomedicine, organizational projects.But, about the research of chiral hydrogel owing to starting late, also do not obtain the enough attention of people.
The preparation of current chiral hydrogel mainly carrys out synthesis of chiral micro-molecular hydrogel by chirality Small molecular (comprising carbohydrate derivative, amino acid, polypeptide analog derivative, dendrimer etc.) as gelator.Plasma chirality mainly refers to has chirality optical signalling in the position at plasma absorption peak.The research of current plasma chirality mainly concentrates on and utilizes noble metal nanometer material (as gold, silver nano particle) to build chirality assembly.
The present invention is on the basis of existing hydrogel, introduces noble metal nanometer material, obtains the hydrogel with plasma chirality by self assembly.
Summary of the invention
The object of this invention is to provide a kind of preparation method with the hydrogel of plasma chirality.
Technical scheme of the present invention: a kind of preparation method with the hydrogel of plasma chirality, comprises the following steps:
(1) preparation of the noble metal nanometer material of modification: be described for nanogold particle, first utilize reduction of sodium citrate legal system for the nanogold particle AuNP of particle diameter at 12nm: by 50mL mass fraction be 1% aqueous solution of chloraurate be heated to boiling, under fast stirring, the mass fraction adding rapidly 1.2mL is wherein the sodium citrate aqueous solution of 1%, continue to add thermal agitation, until finally obtain the solution of claret, stop heating, namely obtain nano-Au solution;
The sodium hydroxide solution of 1mol/L is utilized to regulate the pH of above-mentioned prepared nano-Au solution, its final pH is made to be 11, then a certain amount of 11-sulfydryl alkanoic acid 11-MUA is added wherein, its ultimate density controls as 0.1mg/mL, after the hatching of 6h, namely obtain the nanogold particle AuNP-MUA of 11-MUA protection;
By the centrifugal 30min of above-mentioned system 8000 r/min, remove supernatant, by resuspended with the sodium-chloride water solution of 1mmol/L for precipitation, then PEI (PEI) is added, it is 1 mg/mL that its ultimate density controls, after hatching 24h, and the centrifugal 30min of 8000 r/min, remove supernatant, resuspended with water, once centrifugal again with same condition, remove supernatant, add water resuspended, the concentration controlling final modified Nano gold grain AuNP-MUA-PEI is 10 nmol/L;
(2) preparation of the hydrogel of plasma chirality
The preparation of the L-type glutamic acid Fmoc-L-Glu of 9-fluorenylmethyloxycarbonyl protection: the L-type glutamic acid taking 2 mmol is dissolved in the aqueous sodium carbonate of 15mL, again under condition of ice bath, 15mL adds containing the dioxane solution of 3mmol fluorenes methoxy dicarbonyl chloride, this mixture is stirring reaction 24h at room temperature, then 30mL ethyl acetate is added, be neutral with salt acid for adjusting pH, with extraction into ethyl acetate 2 times, the extract of 2 times is collected, with anhydrous sodium sulfate drying, evaporation and concentration under vacuum, obtains white solid, i.e. Fmoc-L-Glu;
Take Fmoc-L-Glu and the L-type lysine L-Lys of equimolar amounts, add the ultra-pure water of certain volume wherein, heating makes it dissolve, then the noble metal nanometer material AuNP-MUA-PEI of the modification of above-mentioned preparation is added wherein, the concentration of control AuNP-MUA-PEI is the concentration of 1-5 nmol/L, Fmoc-L-Glu and L-Lys is respectively 0.1-1 mol/L, and heating makes it dissolve, to be cooled after room temperature, namely define the hydrogel with plasma chirality.
Beneficial effect of the present invention: the present invention is on the basis of existing hydrogel, introduces noble metal nanometer material, obtains the hydrogel with plasma chirality by self assembly.
Accompanying drawing explanation
Circle two spectrum of the hydrogel of the nano-golden particle-containing of Fig. 1 prepared by embodiments of the invention 1.
Circle two spectrum of the hydrogel of the nano-golden particle-containing of Fig. 2 prepared by embodiments of the invention 2.
Detailed description of the invention
Embodiment 1
(1) preparation of nanogold particle and modification
First utilize reduction of sodium citrate legal system for the nanogold particle (AuNP) of particle diameter at about 12nm: by 50mL mass fraction be 1% aqueous solution of chloraurate be heated to boiling, under fast stirring, the mass fraction adding rapidly 1.2mL is wherein the sodium citrate aqueous solution of 1%, continue to add thermal agitation, until finally obtain the solution of claret, stop heating, namely obtain nanogold particle solution.
Utilize the sodium hydroxide solution of 1mol/L to regulate the pH of above-mentioned prepared nano-Au solution, make its final pH be 11, then add a certain amount of 11-sulfydryl alkanoic acid (11-MUA) wherein, it is 0.1 mg/mL that its ultimate density controls.After the hatching of 6h, namely obtain the nanogold particle (AuNP-MUA) of 11-MUA protection.
By centrifugal for above-mentioned system (with the centrifugal 30min of 8000r/min), remove supernatant, by resuspended with the sodium-chloride water solution of 1mmol/L for precipitation, then add PEI, it is 1 mg/mL that its ultimate density controls.After hatching 24 hours, centrifugal (centrifugal 30 min of 8000r/min) remove supernatant, resuspended with water, once centrifugal again with same condition, and remove supernatant, add water resuspended, the concentration controlling final nanogold particle AuNP-MUA-PEI is 10 nmol/L.
(2) preparation of the hydrogel of plasma chirality
The preparation of the L-type glutamic acid Fmoc-L-Glu of 9-fluorenylmethyloxycarbonyl protection: the L-type glutamic acid taking 2 mmol is dissolved in the aqueous sodium carbonate of 15mL; again under condition of ice bath; 15mL adds containing the dioxane solution of 3mmol fluorenes methoxy dicarbonyl chloride; this mixture is stirring reaction 24h at room temperature; then 30mL ethyl acetate is added; be neutral with salt acid for adjusting pH; with extraction into ethyl acetate 2 times; the extract of 2 times is collected; with anhydrous sodium sulfate drying; evaporation and concentration under vacuum, obtains white solid, i.e. Fmoc-L-Glu.
Take the L-type lysine L-Lys of Fmoc-L-Glu and the 0.1mmol of 0.1mmol, add 900 μ L ultra-pure waters wherein, heating makes it dissolve, then the AuNP-MUA-PEI solution of the above-mentioned preparation of 100 μ L is added wherein, heating makes it dissolve, to be cooled after room temperature, namely define the hydrogel with plasma chirality.
The atomic force microscope phenogram of the hydrogel of the nano-golden particle-containing prepared by embodiment 1 that the sixth of the twelve Earthly Branches obtains, owing to being colored dark figure, omission of can only giving up what one treasures in this patent, the sign of its circle two spectrum is shown in Fig. 1.
Embodiment 2
(1) preparation of nanogold particle and modification
Concrete steps are identical with embodiment 1.
(2) containing the preparation of the plasma chiral hydrogel of nm of gold
The preparation of the L-type glutamic acid Fmoc-L-Glu of 9-fluorenylmethyloxycarbonyl protection: the L-type glutamic acid taking 2 mmol is dissolved in the aqueous sodium carbonate of 15mL; again under condition of ice bath; 15mL adds containing the dioxane solution of 3mmol fluorenes methoxy dicarbonyl chloride; this mixture is stirring reaction 24h at room temperature; then 30mL ethyl acetate is added; be neutral with salt acid for adjusting pH; with extraction into ethyl acetate 2 times; the extract of 2 times is collected; with anhydrous sodium sulfate drying; evaporation and concentration under vacuum, obtains white solid, i.e. Fmoc-L-Glu.
Take the L-type lysine L-Lys of Fmoc-L-Glu and the 1mmol of 1mmol, add 800 μ L ultra-pure waters wherein, heating makes it dissolve, then the AuNP-MUA-PEI solution of the above-mentioned preparation of 200 μ L is added wherein, heating makes it dissolve, to be cooled after room temperature, namely define the hydrogel with plasma chirality.
The sign of circle two spectrum of the chiral hydrogel of gained nano-golden particle-containing is shown in Fig. 2.
Claims (1)
1. there is a preparation method for the hydrogel of plasma chirality, it is characterized in that comprising the following steps:
(1) preparation of modified Nano gold grain: first utilize reduction of sodium citrate legal system for the nanogold particle AuNP of particle diameter at 12nm: by 50mL mass fraction be 1% aqueous solution of chloraurate be heated to boiling, under fast stirring, the mass fraction adding rapidly 1.2mL is wherein the sodium citrate aqueous solution of 1%, continue to add thermal agitation, until finally obtain the solution of claret, stop heating, namely obtain nano-Au solution;
The sodium hydroxide solution of 1mol/L is utilized to regulate the pH of above-mentioned prepared nano-Au solution, its final pH is made to be 11, then a certain amount of 11-sulfydryl alkanoic acid 11-MUA is added wherein, its ultimate density controls as 0.1mg/mL, after the hatching of 6h, namely obtain the nanogold particle AuNP-MUA of 11-MUA protection;
By the centrifugal 30min of above-mentioned system 8000 r/min, remove supernatant, by resuspended with the sodium-chloride water solution of 1mmol/L for precipitation, then PEI PEI is added, it is 1 mg/mL that its ultimate density controls, after hatching 24h, and the centrifugal 30min of 8000 r/min, remove supernatant, resuspended with water, once centrifugal again with same condition, remove supernatant, add water resuspended, the concentration controlling final modified Nano gold grain AuNP-MUA-PEI is 10 nmol/L;
(2) preparation of the hydrogel of plasma chirality
The preparation of the L-type glutamic acid Fmoc-L-Glu of 9-fluorenylmethyloxycarbonyl protection: the L-type glutamic acid taking 2 mmol is dissolved in the aqueous sodium carbonate of 15mL, under condition of ice bath, 15mL adds containing the dioxane solution of 3mmol fluorenes methoxy dicarbonyl chloride, this mixture is stirring reaction 24h at room temperature, then 30mL ethyl acetate is added, be neutral with salt acid for adjusting pH, with extraction into ethyl acetate 2 times, the extract of 2 times is collected, with anhydrous sodium sulfate drying, evaporation and concentration under vacuum, obtains white solid, i.e. Fmoc-L-Glu;
Take Fmoc-L-Glu and the L-type lysine L-Lys of equimolar amounts, add the ultra-pure water of certain volume wherein, heating makes it dissolve, then the noble metal nanometer material AuNP-MUA-PEI of the modification of above-mentioned preparation is added wherein, the concentration of control AuNP-MUA-PEI is the concentration of 1-5 nmol/L, Fmoc-L-Glu and L-Lys is respectively 0.1-1mol/L, and heating makes it dissolve, to be cooled after room temperature, namely define the hydrogel with plasma chirality.
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| CN102558422A (en) * | 2011-12-15 | 2012-07-11 | 天津工业大学 | Porous pH-sensitive P(AAc-co-AAPheEt) chiral hydrogel |
| CN102627723A (en) * | 2012-04-09 | 2012-08-08 | 天津工业大学 | Temperature response type chiral polymer hydrosol with branched chain structure |
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| CN102558422A (en) * | 2011-12-15 | 2012-07-11 | 天津工业大学 | Porous pH-sensitive P(AAc-co-AAPheEt) chiral hydrogel |
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