CN105219386A - A kind of preparation method of carbon quantum dot of no cytotoxicity of unprotect gas - Google Patents
A kind of preparation method of carbon quantum dot of no cytotoxicity of unprotect gas Download PDFInfo
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- CN105219386A CN105219386A CN201510749888.3A CN201510749888A CN105219386A CN 105219386 A CN105219386 A CN 105219386A CN 201510749888 A CN201510749888 A CN 201510749888A CN 105219386 A CN105219386 A CN 105219386A
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Abstract
The present invention relates to a kind of preparation method of carbon quantum dot of no cytotoxicity of unprotect gas, comprising: by Sodium Glutamate high-temperature calcination, obtain carbon point powder; Carbon point is dissolved, sonic oscillation, filter, dry; Dissolved by the product of drying, dialysis, to obtain final product.Preparation method of the present invention is easy and simple to handle, and without the need to shielding gas protection, without the need to condition of high voltage, environmental protection, is easy to suitability for industrialized production.The advantage such as the quantum dot that method of the present invention prepares has no cytotoxicity, good biocompatibility, quantum yield is high, fluorescence property is excellent (the pH characteristic of fluorescent stability, unglazed nictation and excellence), size distribution is homogeneous, monodispersity is good.
Description
Technical field
The invention belongs to the preparation method field of carbon quantum dot, particularly a kind of preparation method of carbon quantum dot of no cytotoxicity of unprotect gas.
Background technology
In recent years, because tradition provides the toxicity of fluorescence dye and traditional semiconductor-quantum-point self to be difficult to accomplish truly to be applied in the middle of actual medical indicia and detection.Even be applied in biomarker and scientific research material, the limiting quantity of interpolation is also only just beyond 1 micrograms per millilitre rank, and so few addition can not meet the needs of mark substantially.Therefore, increasing research starts to pay close attention to inorganic non-metallic carbon granule quantum dot.First, compared with traditional organic fluorescent dye, inorganic non-metallic carbon granule quantum dot not only maintains the absorb light spectrum width of conventional metals quantum dot and continuous print advantage, and has very strong bleach-resistant characteristic, that is, stability of photoluminescence is high.Secondly, compared with metal quantum point, inorganic non-metallic carbon granule quantum dot has the advantage that excitation band is continuous and wider wavelength of transmitted light is stable, and have good biocompatibility and unglazed nictation phenomenon etc. advantage.The more important thing is, the hypotoxicity of carbon quantum dot be other biological marker incomparable, it can use when addition is very large, is enough to obtain perfect biomarker figure.Therefore, the most excellent material of the inorganic non-metallic carbon granule quantum dot current research application aspect such as biomarker, biological detection, bioprobe just.
The synthetic method of current inorganic non-metallic carbon quantum dot mainly contains two kinds, a kind of is synthetic method from top to bottom: pulverize carbon source, make it effectively luminous by the mode of polymer surfaces passivation, mainly comprise arc discharge method, laser method, electrochemical process, mechanical disintegration, ball milling or chemical oxidation.Although carbon point size uniformity prepared by this method is higher, consume energy too high, the carbon point fluorescent yield that except laser burns method prepared by additive method is all lower.Another method is synthetic method from top to bottom: pyrolysis or the suitable precursor of carbonization directly synthesize fluorescent carbon quantum dot, comprises oxidation or etch, pyrolysis organism method, microwave process for synthesizing, ultrasonic method, the doping method of ashes.But the major part in these methods is all that to there is energy consumption too high, contaminate environment, the shortcomings such as preparation condition is harsh.Due to these defects, be difficult to the green industrialized production realizing carbon quantum dot.Therefore, find that a kind of working condition is simple, environmental protection, the raw material method simultaneously preparing again the product of high-quality that is easy to get is quite significant.
Preparing fluorescent carbon point by the method for high temperature pyrolysis is a kind of more popular fluorescent carbon point preparation method.Currently reported, prepare fluorescent carbon point by each seed amino acid of microwave-heating, but there is microwave temperature uncontrollable (there is local hot spots) and the shortcoming such as fluorescence efficiency is not too high.Other prepares the existence often needing shielding gas in the report of carbon quantum dot by pyrolysis organism, this is not only the input adding production cost, and improves production risk.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of carbon quantum dot of no cytotoxicity of unprotect gas, and the method is simple and easy to do, and cost is lower, is easy to suitability for industrialized production.
The preparation method of the carbon quantum dot of the no cytotoxicity of a kind of unprotect gas of the present invention, comprising:
(1) by Sodium Glutamate high-temperature calcination, carbon point powder is obtained; Wherein, the temperature of calcining is 200 ~ 500 DEG C, and the time of calcining is 10min ~ 2.5h;
(2) carbon point in step (1) is dissolved, sonic oscillation, filter, dry;
(3) dissolved by the product of drying in step (2), dialysis, obtains the carbon quantum dot of no cytotoxicity.
The source of described step (1) Glutamic Acid sodium is monosodium glutamate.
Described step is dissolved as dissolve with ethanol or water dissolution in (2).
In described step (2), during calcining, temperature rise rate is 10 DEG C/min.
In described step (2), the time of sonic oscillation is 10 ~ 60min.
Be filtered into Medium speed filter paper in described step (2) to filter.
In described step (2), bake out temperature is 40 ~ 90 DEG C.
In described step (3), dialysis is the 12h that dialyses with 3000Da ~ 3500Da dialysis membrane.
Using amino acid salts in the present invention, i.e. Sodium Glutamate, is Carbon and nitrogen sources, and under inert-free gas protection hot conditions, a step completes carbonization and doping; And in the carbon point of preparation, introduce a certain amount of Na atom and O atom, thus improve the fluorescence efficiency of product.Belong to industrial goods because cheaper starting materials is easy to get, working condition without the need to high pressure and shielding gas, without the need to causing dirty solvent, so the method that this patent provides is easy to the green industrialized production realizing carbon quantum dot.Pyrolysis product is by after separation and purification dialysis treatment, and the carbon granule quantum dot obtained has no cytotoxicity, and quantum yield is high, and granular size is homogeneous, unglazed nictation phenomenon, the plurality of advantages such as fluorescent stability is high.These advantages are that the Sodium Glutamate carbon quantum dot prepared under unprotect gas condition is laid a good foundation in the application of the tradition such as life science, analysis science, Materials science, immune medical science, inspection and quarantine and emerging field.
beneficial effect
(1) preparation method of the present invention is simple to operation, and temperature requirement is not high, reproducible, and cost is low, the shelf time long (lucifuge is less demanding), is easy to suitability for industrialized production;
(2) quantum dot that method of the present invention obtains has that no cytotoxicity, good biocompatibility, quantum yield are high (maximumly reaches 51.5%, with 0.05M sulphuric acid soln configuration Quinine Sulphate Di HC standardized solution, diluting soln when being less than 0.05 with its excitation wavelength 313nm and 338nm place ultraviolet absorptivity, for standard reference solution, calculates quantum yield), fluorescence property excellence (the pH characteristic of fluorescent stability, unglazed nictation and excellence), the advantage such as size distribution is homogeneous, monodispersity is good.
Accompanying drawing explanation
Fig. 1 is preparation method's schema that embodiment 1 pyrolysis method prepares inorganic non-metallic carbon granule quantum dot;
Fig. 2 is the transmission electron microscope picture that embodiment 3 pyrolysis method prepares inorganic non-metallic carbon granule quantum dot;
Fig. 3 is the X-ray diffractogram that embodiment 3 pyrolysis method prepares inorganic non-metallic carbon granule quantum dot;
Fig. 4 is that embodiment 3 pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, the MTT cell toxicity test done as raw material and cellular form difference figure; A, b, c, d are respectively, control group, minimum concentration carbon point, maximum concentration carbon point cellular form figure and cytotoxicity histogram;
Fig. 5 is that embodiment 2 pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, and calcination time is 30min, without N
2under protection, calcining temperature is respectively uv-absorbing and the fluorescence compound collection of illustrative plates of 200 DEG C, 300 DEG C, 400 DEG C and 500 DEG C;
Fig. 6 is that embodiment 2 and comparative example 2 pyrolysis method prepare inorganic non-metallic carbon granule quantum dot, without N
2and have N
2under protection, calcining temperature is respectively the fluorescent intensity contrast figure of 200 DEG C, 300 DEG C, 400 DEG C and 500 DEG C.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) load in monkey by 2g Sodium Glutamate sample (general monosodium glutamate), without the need to grinding, calcine 50min at 450 DEG C, temperature rise rate is 10 DEG C/min, carries out calcining carbonization and doping process;
(2) by calcining the product obtained, scrape from crucible, after grinding fully, with anhydrous alcohol solution, sonic oscillation 20min, after filtering with Medium speed filter paper, 60 DEG C of oven dry are stand-by;
(3) dissolve desciccate in (2) with a small amount of distilled water, with 3000Da ~ 3500Da dialysis membrane dialysis 12h, extracellular fluid dialysis is liquid product, both obtains solid phase prod after drying.
Fig. 1 is preparation method's schema.The products configuration that embodiment 1 and comparative example 1 obtain becomes 1mg/mL carbon point solution, and with Quinine Sulphate Di HC solution for standard, tests uv-absorbing and fluorescence intensity respectively.Thus draw the quantum yield of this carbon point.
Embodiment 2
(1) load in monkey by 2g Sodium Glutamate sample (general monosodium glutamate), without the need to grinding, calcination time is 30min, and temperature rise rate is 10 DEG C/min, without N
2under protection, calcining temperature is respectively 200 DEG C, 300 DEG C, 400 DEG C and 500 DEG C, carries out calcining carbonization and doping process;
(2) by calcining the product obtained, scraping from crucible, after grinding fully, being dissolved in water, sonic oscillation 20min, after filtering with Medium speed filter paper, get filtrate and again filter with 0.22 μm of water system filter membrane.
Fig. 5 is that pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, and calcination time is 30min, without N
2under protection, calcining temperature is respectively uv-absorbing and the fluorescence compound collection of illustrative plates of 200 DEG C, 300 DEG C, 400 DEG C and 500 DEG C.As can be seen from the figure, when calcination time is identical, calcining temperature is that the fluorescence intensity of the product of 400 DEG C is the highest.Fig. 6 is that pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, without N
2and have N
2under protection, calcining temperature is respectively the fluorescent intensity contrast figure of 200 DEG C, 300 DEG C, 400 DEG C and 500 DEG C.Can find out, remove N
2the product fluorescence intensity obtained after protection is higher, so produce the characteristic that Sodium Glutamate carbon quantum dot not only simplifies experiment condition but also improve product under unprotect gas.
Embodiment 3
(1) load in monkey by 2g Sodium Glutamate sample (general monosodium glutamate), without the need to grinding, calcine 30min at 400 DEG C, temperature rise rate is 10 DEG C/min, carries out calcining carbonization and doping process;
(2) by calcining the product obtained, scrape from crucible, after grinding fully, with anhydrous alcohol solution, sonic oscillation 20min, after filtering with Medium speed filter paper, 60 DEG C of oven dry are stand-by;
(3) dissolve desciccate in (2) with a small amount of distilled water, with 3000Da ~ 3500Da dialysis membrane dialysis 12h, extracellular fluid dialysis is liquid product, both obtains solid phase prod after drying.
Fig. 2 is the transmission electron microscope picture that pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, and average particle size is about 6.78nm.Fig. 3 is the X-ray diffractogram that pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, and the graphite base peak position of diffraction peak and standard is basically identical (natural characteristics of carbon point imperfections graphite crystalline structure).Fig. 4 is that embodiment 3 pyrolysis method prepares inorganic non-metallic carbon granule quantum dot, the MTT cell toxicity test done as raw material and cellular form difference figure, can find out that the form of cell under quite high carbon point concentration is complete and present Normocellular fusiformis, cytotoxicity is less; Wherein, a, b, c, d are respectively control group, minimum concentration carbon point, maximum concentration carbon point cellular form figure and cytotoxicity histogram.
Comparative example 1
(1) load in monkey by 2g Sodium Glutamate sample (general monosodium glutamate), without the need to grinding, calcine at 200 ~ 500 DEG C, temperature rise rate is 10 DEG C/min, has N
2under protection, calcination time is respectively 0.5h, 1h, 1.5h, 2h and 2.5h, carries out calcining carbonization and doping process;
(2) by calcining the product obtained, scraping from crucible, after grinding fully, being dissolved in water, sonic oscillation 20min, after filtering with Medium speed filter paper, get filtrate and again filter with 0.22 μm of water system filter membrane.
Comparative example 2
(1) load in monkey by 2g Sodium Glutamate sample (general monosodium glutamate), without the need to grinding, calcination time is 30min, and temperature rise rate is 10 DEG C/min, has N
2under protection, calcining temperature is respectively 200 DEG C, 300 DEG C, 400 DEG C and 500 DEG C, carries out calcining carbonization and doping process;
(2) by calcining the product obtained, scraping from crucible, after grinding fully, being dissolved in water, sonic oscillation 20min, after filtering with Medium speed filter paper, get filtrate and again filter with 0.22 μm of water system filter membrane.
Claims (6)
1. a preparation method for the carbon quantum dot of the no cytotoxicity of unprotect gas, comprising:
(1) by Sodium Glutamate high-temperature calcination, carbon point powder is obtained; Wherein, the temperature of calcining is 200 ~ 500 DEG C, and the time of calcining is 10min ~ 2.5h;
(2) carbon point in step (1) is dissolved, sonic oscillation, filter, dry;
(3) dissolved by the product of drying in step (2), dialysis, obtains the carbon quantum dot of no cytotoxicity.
2. the preparation method of the carbon quantum dot of the no cytotoxicity of a kind of unprotect gas according to claim 1, is characterized in that, described step is dissolved as dissolve with ethanol or water dissolution in (2).
3. the preparation method of the carbon quantum dot of the no cytotoxicity of a kind of unprotect gas according to claim 1, is characterized in that, in described step (2), during calcining, temperature rise rate is 10 DEG C/min.
4. the preparation method of the carbon quantum dot of the no cytotoxicity of a kind of unprotect gas according to claim 1, is characterized in that, in described step (2), the time of sonic oscillation is 10 ~ 60min.
5. the preparation method of the carbon quantum dot of the no cytotoxicity of a kind of unprotect gas according to claim 1, is characterized in that, is filtered into Medium speed filter paper and filters in described step (2).
6. the preparation method of the carbon quantum dot of the no cytotoxicity of a kind of unprotect gas according to claim 1, is characterized in that, in described step (3), dialysis is the 12h that dialyses with 3000Da ~ 3500Da dialysis membrane.
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| CN107727619A (en) * | 2017-09-11 | 2018-02-23 | 东华大学 | One kind using taurine carbon point be probe to Fe3+Carry out qualitative and quantitative detecting method |
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