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 PDF

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Publication number
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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China
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quantum dot
carbon quantum
fluorescent carbon
preparation
egg
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CN201711004873.XA
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李炳生
余立冬
魏新晶
贺金梅
李丽
陈洪宇
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Harbin Institute of Technology
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Harbin Institute of Technology
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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

A method of fluorescent carbon quantum dot is prepared by predecessor microwave method of egg
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.
CN201711004873.XA 2017-10-25 2017-10-25 A method of fluorescent carbon quantum dot is prepared by predecessor microwave method of egg Pending CN109705856A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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
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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
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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Title
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Cited By (4)

* Cited by examiner, † Cited by third party
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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