CN109705856A - A method of fluorescent carbon quantum dot is prepared by predecessor microwave method of egg - Google Patents
A method of fluorescent carbon quantum dot is prepared by predecessor microwave method of egg Download PDFInfo
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- CN109705856A CN109705856A CN201711004873.XA CN201711004873A CN109705856A CN 109705856 A CN109705856 A CN 109705856A CN 201711004873 A CN201711004873 A CN 201711004873A CN 109705856 A CN109705856 A CN 109705856A
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Abstract
A method of fluorescent carbon quantum dot being prepared by predecessor of egg, belongs to fluorescent carbon quantum dot preparation field.Using natural biological materials egg as carbon source, yolk and albumen are separated using egg white separator, water-soluble fluorescent carbon point is made by microwave method respectively.Raw material of the present invention easily takes, low in cost, and synthesis step is simple, quick obtaining, easy to operate, it can be achieved that large-scale production, environmentally protective, without adding toxic chemical.Result of study shows that the fluorescent carbon quantum dot good water solubility obtained, fluorescence intensity are high, cell imaging, biomarker, catalysis engineering and biosensor, disease surveillance and in terms of show wide application prospect.
Description
Technical field
The invention belongs to fluorescent carbon quantum dot preparation fields, and in particular to one kind prepares glimmering using egg as predecessor microwave method
The method of light carbon quantum dot.
Background technique
Carbon constitutes basic structural unit of life entity, such as amino acid, polysaccharide, protein etc., it can be said that
Bright carbon has good biocompatibility and biological safety in vivo.Xu in 2004 et al., it is single separating and purifying
Carbon nano-particles are chanced on during wall carbon nano tube, and their continuous nano-scale particles in the research in later period
Photoluminescent property attempts to develop a kind of emerging fluorescent nano material.Sun in 2006 et al. has named this fluorescent carbon to receive for the first time
Rice corpuscles be carbon quantum dot (Carbon Dots, CDs), and propose by surface purify method can effectively enhance
The fluorescent emission intensity of fluorescent carbon quantum dot.Carbon dots refer to size generally in 10nm carbon nano-particle below.Because of its surface band
There is functional group abundant, such as-OH, the hydrophilic radicals such as-COOH, C=O, and there is good water solubility.By last decade to carbon
The research of quantum dot, the preparation method of carbon quantum dot are generally summarized as two kinds, respectively method from top to bottom, from bottom to top method.Tool
Body mainly has burning/high temperature method, hydro-thermal method, strong acid method for oxidation, microwave method, solution chemistry synthetic method, plasma synthesis method
Deng.However these methods usually all can be using Organic Compounds as carbon source, synthesis condition is harsh, complex steps, and is closing
Toxic reagent can be added during at carbon quantum dot.
Thus researchers, which are exploring always with carbon source environmentally protective, inexpensive, from a wealth of sources, synthesizes carbon quantum dot,
And some achievements is had been achieved with, such as use hay, coffee, pomelo peel, orange juice etc. and successfully prepare carbon amounts as predecessor
Sub- point.But there are some defects for the carbon quantum dot of these sources preparation.For example, launch wavelength is shorter, quantum yield is low, water-soluble
Property is poor, fluorescence intensity is low etc., limits the bigger application of carbon quantum dot.Albumen and yolk in egg contain a large amount of albumen
Matter, mainly albumen egg and vitellin, furthermore containing the largely ingredient beneficial to human body: vitamin A, vitamin D, iron,
The minerals such as phosphorus, sulphur and calcium.The present invention selects natural biomass egg from a wealth of sources, cheap and easy to get as predecessor, realizes
Simple extensive rapidly synthesizing water-solubility is good, good light stability, and is expected to be used for cell marking and cell imaging.
Summary of the invention
The disadvantage that the synthetic yield that the present invention is directed to traditional quantum dot is low, photostability is poor, fluorescence intensity is weak, with egg
Albumen and yolk prepare carbon quantum dot using microwave method, this method streamline operation prepares high yield respectively as carbon source
The fluorescent carbon point that rate, photostability be strong, good water solubility, fluorescence intensity are high, and system is carried out to the fluorescent characteristic of this carbon quantum dot
Research.
To achieve the above object, the technical solution adopted by the present invention is as follows:
In the method that egg prepares fluorescent carbon quantum dot as predecessor, the method is microwave method.Specific preparation step is such as
Under:
Step 1: obtaining a certain amount of albumen and yolk using protein separator respectively, stir evenly respectively, is put into and adds
In the micro-wave oven of 500~1000W of thermal power, heating time is 20~40min, and solution colour changes, faded to by liquid black
Brown solid is cooled to room temperature;
Step 2: dark brown solid is ground, and carries out 2~3d of mixing with deionized water, then in centrifugation rate
Differential centrifugation is carried out for 2000~22000r/min, 10~40min is centrifuged, takes supernatant liquor, is 0.22 μm in the aperture of filter membrane
In the case of filtered, obtain clear liquid;
Step 3: the use of the molecular cut off of bag filter is 1000~14000Da, dialysis is carried out 3~6 days to clear liquid.Most
Freeze-drying is carried out 2~3 days under the conditions of -20 DEG C~-60 DEG C afterwards, obtains carbon quantum dot powder.
The present invention for the prior art the utility model has the advantages that using natural biomass egg as predecessor, it is from a wealth of sources, honest and clean
Valence is easy to get, method is simple and easy, safe ready, environmentally protective, without adding toxic chemical, may be implemented quickly and easily
Extensive synthesis fluorescence intensity is high, stability of photoluminescence is good, good water solubility fluorescent carbon quantum dot.
Detailed description of the invention
Fig. 1 is fluorescence spectra of the fluorescent carbon point of the preparation of embodiment 1 under different excitation wavelengths;
Fig. 2 is the uv absorption spectra of fluorescent carbon point prepared by embodiment 1;
Fig. 3 is the HRTEM figure of fluorescent carbon point prepared by embodiment 1;
Fig. 4 is fluorescence spectra of the fluorescent carbon point of the preparation of embodiment 2 under different excitation wavelengths;
Fig. 5 is the uv absorption spectra of fluorescent carbon point prepared by embodiment 2.
Specific embodiment
Following embodiment is some citings of the invention, should not be seen as limitation of the invention, all to the present invention
Technical solution is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered at this
In the protection scope of invention.
Embodiment 1: that present embodiment is recorded is the method for preparing fluorescent carbon quantum dot as predecessor using albumen, the side
Tagmeme microwave method, specific preparation process is as follows:
Step 1: being uniformly mixing to obtain yellow solution for 100mL protein solution, and solution is put into 700W micro-wave oven and is added
Hot 25min becomes dark brown solid, cooled to room temperature from yellow solution;
Step 2: dark brown solid is ground, and 500mL deionized water is added and forms turbid, persistently stirs 48h, will
Turbid, which is placed in a centrifuge, to be successively centrifuged by 2000~22000r/min centrifugation rate, and centrifugation time is 10~30min,
Its supernatant, then the filtering with microporous membrane that via hole diameter is 0.22 μm are taken, clear liquid is obtained;
Step 3: the use of the molecular cut off of bag filter is 3500Da, dialysis is carried out 3~6 days to clear liquid, obtains carbon quantum
Point solution, and the solution be freeze-dried to 2~3 days under the conditions of -20 DEG C~-60 DEG C to get carbon quantum dot powder is arrived.
Fluorescence property test is carried out to the water-solubility fluorescent carbon quantum dot prepared in the present embodiment with sepectrophotofluorometer,
Fig. 1 is obtained, as can be seen from Figure 1 as excitation wavelength increases, Red Shift Phenomena occurs for the absorption maximum summit of emission spectrum, embodies
Emission spectrum has excitation wavelength dependency characteristic out.When excitation wavelength is 340nm, maximum emission wavelength 415nm.With ultraviolet
Spectrophotometer carries out ultra-violet absorption spectrum test, obtained purple to the water-solubility fluorescent carbon quantum dot of the preparation in the present embodiment
Outer absorption spectrum is as shown in Fig. 2, it can be seen from the figure that the fluorescent carbon quantum dot solution of this method synthesis has one at 270nm
A weak absorbing peak, this is by phenyl ring sp2Caused by π-π * transition of hydridization.With transmission electron microscope to being made in the present embodiment
Standby water-solubility fluorescent carbon quantum dot carries out electron-microscope scanning, obtains Fig. 3, from figure 3, it can be seen that the carbon quantum dot of this method synthesis
It is with good dispersion.
Embodiment 2: that present embodiment is recorded is the method for preparing fluorescent carbon quantum dot as predecessor using yolk, the side
Tagmeme microwave method, specific preparation process is as follows:
Step 1: 100mL yolk solution is uniformly mixing to obtain yellow solution, solution is put into 700W micro-wave oven and is heated
25min becomes dark brown solid, cooled to room temperature from yellow solution;
Step 2 grinds dark brown solid, and 500mL deionized water is added and forms turbid, persistently stirs 48h, will be turbid
Liquid, which is placed in a centrifuge, to be successively centrifuged by 2000~22000r/min centrifugation rate, and centrifugation time is 10~30min, is taken
Its supernatant, then the filtering with microporous membrane that via hole diameter is 0.22 μm, obtain clear liquid;
Step 3: the use of the molecular cut off of bag filter is 3500Da, dialysis is carried out 3~6 days to clear liquid, obtains carbon quantum
Point solution, and the solution be freeze-dried to 2~3 days under the conditions of -20 DEG C~-60 DEG C to get carbon quantum dot powder is arrived.
Fluorescence property test is carried out to the water-solubility fluorescent carbon quantum dot prepared in the present embodiment with sepectrophotofluorometer,
Fig. 4 is obtained, as can be seen from Figure 4 as excitation wavelength increases, Red Shift Phenomena occurs for the absorption maximum summit of emission spectrum, embodies
Emission spectrum has excitation wavelength dependency characteristic out.When excitation wavelength is 340nm, maximum emission wavelength 425nm.With ultraviolet
Spectrophotometer carries out ultra-violet absorption spectrum test, obtained purple to the water-solubility fluorescent carbon quantum dot of the preparation in the present embodiment
Outer absorption spectrum is as shown in figure 5, it can be seen from the figure that the fluorescent carbon quantum dot solution of this method synthesis has one at 280nm
A weak absorbing peak, this is by phenyl ring sp2Caused by π-π * transition of hydridization.
Claims (5)
1. a kind of method for preparing fluorescent carbon quantum dot as predecessor using egg, it is characterised in that: the preparation method is that microwave
Method, specific preparation step are as follows: obtain a certain amount of albumen and yolk respectively using protein separator, stir evenly, put respectively
Entering and heats certain time in the micro-wave oven of certain power, solution fades to dark brown solid by faint yellow, yellow color liquid respectively,
It is cooled to room temperature, then grinds solid, be mixed with deionized water, carry out differential centrifugation, take supernatant liquor,
It is filtered using the filter membrane that aperture is 0.22 μm, goes supernatant liquor to dialyse, finally under the conditions of -20 DEG C~-60 DEG C, be freeze-dried
It is dried in machine 2~3 days, obtains carbon quantum dot powder.
2. preparation method according to claim 1, it is characterised in that: the microwave reaction time is 10~40min.
3. preparation method according to claim 1, it is characterised in that: microwave reaction power is 500~1000W.
4. preparation method according to claim 1, it is characterised in that: revolving speed is 2000~22000r/ when differential centrifugation
Min, centrifugation time are respectively 10~40min.
5. preparation method according to claim 1, it is characterised in that: the molecular cut off of bag filter be 1000~
14000Da, dialysis time are 3~6 days.
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Cited By (3)
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CN110715915A (en) * | 2019-11-06 | 2020-01-21 | 东北师范大学 | Method for detecting ferric ions based on carbon quantum dots prepared from egg white |
CN112670477A (en) * | 2020-12-24 | 2021-04-16 | 江西师范大学 | Vanadium nitride quantum dot in-situ implanted carbon sphere composite material, preparation method thereof and sodium storage application |
CN116970388A (en) * | 2023-07-27 | 2023-10-31 | 北京理工大学 | Carbon quantum dot fluorescent probe based on plant fructus xanthil and preparation method and application thereof |
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CN103387219A (en) * | 2013-07-22 | 2013-11-13 | 苏州大学 | A preparation method for water-soluble multicolor carbon quantum points by microwave radiation |
CN103588189A (en) * | 2013-07-04 | 2014-02-19 | 上海交通大学 | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots |
CN105038781A (en) * | 2015-04-01 | 2015-11-11 | 河南师范大学 | Method of one-step synthesizing fluorescent carbon dots with corncob as carbon source |
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CN103588189A (en) * | 2013-07-04 | 2014-02-19 | 上海交通大学 | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots |
CN103387219A (en) * | 2013-07-22 | 2013-11-13 | 苏州大学 | A preparation method for water-soluble multicolor carbon quantum points by microwave radiation |
CN105038781A (en) * | 2015-04-01 | 2015-11-11 | 河南师范大学 | Method of one-step synthesizing fluorescent carbon dots with corncob as carbon source |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110715915A (en) * | 2019-11-06 | 2020-01-21 | 东北师范大学 | Method for detecting ferric ions based on carbon quantum dots prepared from egg white |
CN112670477A (en) * | 2020-12-24 | 2021-04-16 | 江西师范大学 | Vanadium nitride quantum dot in-situ implanted carbon sphere composite material, preparation method thereof and sodium storage application |
CN112670477B (en) * | 2020-12-24 | 2023-04-18 | 江西师范大学 | Vanadium nitride quantum dot in-situ implanted carbon sphere composite material, preparation method thereof and sodium storage application |
CN116970388A (en) * | 2023-07-27 | 2023-10-31 | 北京理工大学 | Carbon quantum dot fluorescent probe based on plant fructus xanthil and preparation method and application thereof |
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