CN104177540B - The preparation method of the fluorescent type temperature intelligent response sensor based on gold nanoclusters - Google Patents
The preparation method of the fluorescent type temperature intelligent response sensor based on gold nanoclusters Download PDFInfo
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Abstract
The present invention relates to the preparation method of the fluorescent type temperature intelligent response sensor based on gold nanoclusters. Do you in the present invention, select the coated Au nano-cluster (AuBSA of bovine serum albumin(BSA)? NCs), as the signal source that good fluorescence property is provided, poly-N-isopropyl acrylamide (PNIPAM) conduct can be to the macromolecular material of variation of ambient temperature intelligent response. Prepare gained Au/PNIPAM hybridized hydrogel fluorescence intensity can with environment temperature raise or reduce and reversibly weaken or strengthen, thereby develop into fluorescent type temperature intelligent response sensor; Advantage of the present invention: this preparation method not only process is simple, and cost-saving. Is the step of technology of preparing as follows: the first synthetic AuBSA with good fluorescence performance? NCs, then mixes with temperature sensitive polymerization single polymerization monomer NIPAM, (25 DEG C) trigger monomer polymerization under the condition coexisting at crosslinking agent, initator. In this process, AuBSA? NCs is embedded in the network structure of PNIPAM, and by good interaction of hydrogen bond between surface group, has formed the Au/PNIPAM hybridized hydrogel with stable fluorescence property.
Description
Technical field
The present invention relates to the technology of preparing of the fluorescent type temperature intelligent response sensor based on gold nanoclusters, particularly normal temperatureUnder, easy fast synthetic Au/PNIPAM hybridized hydrogel, and developed into fluorescent type temperature intelligent response sensor.
Background technology
Intelligent response material is to integrate from detecting (sensing), certainly judgement and the new material from conclusion (processing) function. ItCan imitate life system, and to environmental change perception, response, therefore there is function ability of discovery. Poly-N-isopropyl propyleneAcid amides (PNIPAM) be widely used a kind of temperature intelligent response type polymer (H.G.Schild, Prog.Polym.Sci.,1992,17,163-249; R.Pelton, Adv.ColloidInterfac., 2000,85,1-33). PNIPAM hydrogel dividesHydrophobic group (CH (CH3) 2) in subchain and hydrophilic radical (NHCO-) can temperature influences and that hydrophilic/hydrophobic occurs is flatWeighing apparatus (J.R.Retama, Langmuir, 2007,23,10280-10285), Here it is PNIPAM hydrogel has Thermo-sensitiveBasic reason. In the time that environment temperature changes near lowest critical solution temperature (LCST), can there is body in PNIPAM hydrogelLong-pending change mutually (S.Stephan, Adv.Funct.Mater., 2010,20,3235-3243.), therefore it can be widely used in respectivelyThe field of kind. As: medicine transmission, controlled medicine discharge, Sensor Design (J.M.Weissman, Science, 1996,274,959-963) etc.
The coated gold nanoclusters (AuBSANCs) of bovine serum albumin(BSA) is a kind of emerging nano-luminescent material. Because it is superLittle size, good biocompatibility, near-infrared fluorescent transmitting, the feature such as the narrow and peak shape of emission spectrum is symmetrical (J.PXie,J.Am.Chem.Soc.2009,131,888-889), be just widely used in fluorescence labeling, biomedical imaging, fluorescence biographyThe fields such as sensor design. The present invention relates to the AuBSANCs with good fluorescence performance to be incorporated into PNIPAM water-settingIn glue network structure, thereby gather both advantage, synthetic Au/PNIPAM hybridized hydrogel material. This material both retainedThe temperature sensitive performance of PNIPAM, combine again electricity, the optical characteristics of gold nanoclusters excellence. Preparation involved in the present inventionThe method of Au/PNIPAM hybridized hydrogel, not only process is simple, and cost-saving. In the time that environment temperature raises or reduce,Can impel PNIPAM network structure contraction or expansion, further cause that the fluorescence intensity signals of inner AuNCs reducesOr strengthened, and show and varied with temperature good invertibity and reproducibility. Therefore, this Au/PNIPAM hydridization waterGel rubber material can develop into fluorescent type temperature intelligent response sensor.
Summary of the invention
The object of the invention is, on the basis of above-mentioned technical Analysis, provide a kind of fluorescent type of preparing based on gold nanoclustersThe method of temperature intelligent response sensor. This technology of preparing will have the nano material of high fluorescence property and temperature sensitive response performanceMacromolecule polymer material set is integrated, and has widened the application category of composite. This preparation method's process is simple, syntheticHybridized hydrogel material there is stable fluorescence property, and its fluorescence intensity vary with temperature shown good reversibleProperty.
Technical scheme of the present invention:
Prepare a method for the fluorescent type temperature intelligent response sensor based on gold nanoclusters, using AuNCs as fluorescenceSignal source, using PNIPAM as the intelligent macromolecule polymer that can respond variation of ambient temperature. When monomer, NIPAM sends outWhen raw polymerisation, AuNCs can be evenly embedded in the network structure of polymer. Due to the ox on AuNCs surfaceOn seralbumin, there is amino, can and PNIPAM network structure on amido link between form good hydrogen bond action, thisSample just can prepare the Au/PNIPAM hybridized hydrogel material with stable fluorescence property, specifically comprises the steps:
1) gold nanoclusters (AuBSANCs) is synthetic: after for reaction vessel, chloroazotic acid, ethanol, intermediate water wash successively,First add bovine serum albumin(BSA) (BSA) solution, then add gold chloride (HAuCl4) solution and stir (37 DEG C), after 2 minutes, addA small amount of NaOH (NaOH) aqueous solution, reaction is carried out obtaining AuBSANCs solution after 12h, products therefrom dialysis48h；
2) preparation of Au/PNIPAM hybridized hydrogel: get a certain amount of above-mentioned AuBSANCs solution soluble in water,Add again appropriate monomer NIPA (NIPAM), crosslinking agent N, N '-methylene-bisacrylamide (MBA),Ultrasonic concussion 2min makes Solution Dispersion even. By reaction vessel sealing, and insert the lasting nitrogen 30min that imports of air guide syringe needle,By whole the oxygen in solution Ex-alls. Add subsequently initiator potassium persulfate (KPS) and accelerator N, N, N ', N '-tetra-Methyl ethylenediamine (TEMED), initiated polymerization carries out (25 DEG C) after 3h, can prepare Au/PNIPAM hydridization waterGel.
The concentration of synthetic middle gold chloride (HAuCl4) solution of described gold nanoclusters is 5-20mM, bovine serum albumin(BSA) (BSA)Solution concentration is 30-50mg/mL, and NaOH (NaOH) concentration of aqueous solution is 0.5-1.0mol/L. Gold chloride (HAuCl4)The volume ratio of solution, bovine serum albumin(BSA) (BSA) solution and NaOH (NaOH) solution is 10: 10: 1. DescribedIn Au/PNIPAM hybridized hydrogel synthetic, the concentration of AuNCs solution used is 5mM, and each ratio of reagents used is:The volume ratio of water, gold nanoclusters solution, accelerator (TEMED) is 200: 100: 1; Polymerization single polymerization monomer (NIPAM), initator(KPS), the mass ratio of crosslinking agent (MBA) is 200: 10: 3.
Advantage of the present invention and good effect:
1) fluorescence quantum yield of gold nanoclusters is high, and the transmitting of its red fluorescence has the responsive effect of obvious vision, therefore can doFor preparing the good signal source of sensor. Temperature sensitive to gold nanoclusters and macromolecule intelligent response material is combined, can be its many meritsEnergyization application provides the platform of a sol-gel;
2) PNIPAM is a kind of temperature sensitive macromolecular material with good biocompatibility, and itself and nano-luminescent material are tied mutuallyClose, given its new application prospect.
3) the Au/PNIPAM hybridized hydrogel of synthesized, not only has stable fluorescent emission character, and has shownGood change and the character of reversible variation occurs fluorescence intensity signals with ambient temperature. Therefore, can be developed into fluorescent typeTemperature intelligent response sensor.
Brief description of the drawings
Fig. 1 is AuNCs solution (a), and blank PNIPAM gel (b) and Au/PNIPAM hybridized hydrogel (c) are at visible ray (A)And photo under uviol lamp (B).
Fig. 2 is the normalization fluorescence spectrum figure of AuNCs and Au/PNIPAM hybridized hydrogel.
Fig. 3 be this Au/PNIPAM hybridized hydrogel between 25 DEG C to 43 DEG C, repeatedly heat up-lower the temperature repeatedly circulation time fluorescence intensity becomeChange figure.
Detailed description of the invention
Embodiment:
Prepare a method for the fluorescent type temperature intelligent response sensor based on gold nanoclusters, by causing at normal temperatures listWhen body NIPAM polymerization reaction take place, by even AuNCs embedding and by hydrogen bond action stable bond in polymerIn network structure. Prepare the Au/PNIPAM hybridized hydrogel material with stable fluorescence property, comprised the steps:
1) gold nanoclusters (AuBSANCs) is synthetic: after for reaction vessel, chloroazotic acid, ethanol, intermediate water wash successively,First adding 1mL concentration is bovine serum albumin(BSA) (BSA) solution of 50mg/mL, then to add 1mL concentration be the chlorine of 10mMAuric acid (HAuCl4) solution also stirs (37 DEG C), and after 2 minutes, adding 0.1mL concentration is the NaOH (NaOH) of 1.0mol/LThe aqueous solution, reaction is carried out obtaining AuBSANCs solution after 12h, products therefrom dialysis 48h;
2) preparation of Au/PNIPAM hybridized hydrogel: get the above-mentioned AuBSANCs solution of 1mL (5mM) and be dissolved in 2mLIn water, then add 0.2g monomer NIPA (NIPAM), 0.003g crosslinking agent N, N '-di-2-ethylhexylphosphine oxide propyleneAcid amides (MBA), ultrasonic concussion 2min makes Solution Dispersion even. By reaction vessel sealing, and insert the lasting importing of air guide syringe needleNitrogen 30min, by whole the oxygen in solution Ex-alls. Add subsequently 0.01g initiator potassium persulfate (KPS) and 10 μ L to addSpeed agent TEMED (TEMED), initiated polymerization carries out (25 DEG C) after 3h, can makeThe standby Au/PNIPAM hybridized hydrogel that obtains.
Use with the sepectrophotofluorometer of constant temperature water bath apparatus and measure the Au/PNIPAM hybridized hydrogel of preparing gained,Its maximum emission wavelength place fluorescence intensity is Changing Pattern (sepectrophotofluorometer: Hitachi, day under different ambient temperaturesThis, F-4500 type; Excite slit 10nm, transmitting slit 10nm, excitation wavelength is set in 400nm, at 540-800nmIn scope, record the experimental data of fluorescence emission spectrum, the voltage that photoelectricity training increases pipe is 950V).
Fig. 1 is AuNCs solution (a), and blank PNIPAM gel (b) and Au/PNIPAM hybridized hydrogel (c) are visiblePhoto under light (A) and uviol lamp (B). In figure, show: the fluorescent emission color of original AuNCs solution is redness, blankThe slightly blue-fluorescence transmitting of PNIPAM gel, after Au/PNIPAM hybridized hydrogel forms, its fluorescent emission wavelength blue shift,Show as aubergine fluorescent emission, and in this gel, AuNCs is uniformly dispersed, fluorescent stability is good.
Fig. 2 is the normalization fluorescence spectrum comparison diagram of AuNCs and Au/PNIPAM hybridized hydrogel. In figure, can find out,The fluorescent emission wavelength of AuNCs is about 675nm, and the fluorescent emission wavelength of Au/PNIPAM hybridized hydrogel is about665nm, shows after polymerization, the about 10nm of fluorescent emission wavelength blue shift of AuNCs.
Fig. 3 is this Au/PNIPAM hybridized hydrogel repeatedly heat up-lower the temperature between 25 DEG C to 43 DEG C fluorescence intensity of circulation timeVariation diagram. In figure, can find out, in the time that environment temperature is increased to 43 DEG C, can there is significant reduction in the fluorescence intensity of sensor,In the time that environment temperature is reduced to 25 DEG C, its fluorescence intensity can strengthen again, and in the process of circulating-heating repeatedly-cooling,Fluorescence intensity has shown good varying with temperature and the trend of reversible variation.
Claims (3)
1. a method of preparing the fluorescent type temperature intelligent response sensor based on gold nanoclusters, is characterized in that: adopt oxCoated Au nano-cluster (AuBSANCs) conduct of seralbumin provides the signal source of good fluorescence property, poly-N-isopropylBase acrylamide (PNIPA), as can be to the macromolecular material of environment temperature intelligent response, be prepared the Au/PNIPA hydridization of gainedHydrogel, its fluorescence intensity can raise or reduce and weaken significantly or strengthen with environment temperature, and have good canContrary property, therefore can develop into fluorescent type temperature intelligent response sensor, and preparation process comprises the steps:
1. gold nanoclusters (AuBSANCs) is synthetic: after for reaction vessel, chloroazotic acid, ethanol, intermediate water wash successively, firstAdd bovine serum albumin(BSA) (BSA) solution, then add gold chloride (HAuCl4) solution, and at 37 DEG C stirring reaction 2 minutesAfter add a small amount of NaOH (NaOH) aqueous solution, reaction carry out obtaining AuBSANCs solution after 12h, gained produceThing dialysis 48h;
2. the preparation of Au/PNIPA hybridized hydrogel: get a certain amount of above-mentioned AuBSANCs solution soluble in water, then addEnter appropriate monomer NIPA (NIPA), crosslinking agent N, N '-methylene-bisacrylamide (MBA), ultrasonicConcussion 2min makes Solution Dispersion even, by reaction vessel sealing, and inserts the lasting nitrogen 30min that imports of air guide syringe needle, by moltenThe whole Ex-alls of oxygen in liquid, add initiator potassium persulfate (KPS) and accelerator N, N, N ', N '-tetramethyl subsequentlyEthylenediamine (TEMED), initiated polymerization carries out, after 3h, can preparing Au/PNIPA hybridized hydrogel at 25 DEG C.
2. prepare according to claim 1 the method for the fluorescent type temperature intelligent response sensor based on gold nanoclusters, its spyLevy and be: the concentration of synthetic middle gold chloride (HAuCl4) solution of described AuBSANCs is 5-20mM, bovine serum albuminThe concentration of (BSA) solution is 30-50mg/mL in vain, and the concentration of NaOH (NaOH) solution is 0.5-1.0mol/L, gold chloride(HAuCl4) volume ratio of solution, bovine serum albumin(BSA) (BSA) solution and NaOH (NaOH) solution is 10: 10: 1.
3. prepare according to claim 1 the method for the fluorescent type temperature intelligent response sensor based on gold nanoclusters, its spyLevy and be: in described Au/PNIPA hybridized hydrogel synthetic, the concentration of AuNCs solution used is 5mM, used eachRatio of reagents is: the volume ratio of water, gold nanoclusters solution, accelerator TEMED is 200: 100: 1; Monomer NIPA,The mass ratio of initator KPS, crosslinking agent MBA is 200: 10: 3.
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Application publication date: 20141203 Assignee: SHANXI ZHIDIAN TECHNOLOGY Co.,Ltd. Assignor: Taiyuan University of Technology Contract record no.: X2022140000014 Denomination of invention: Preparation method of fluorescent smart temperature response sensor based on gold nanoclusters Granted publication date: 20160518 License type: Common License Record date: 20221223 |
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