CN106587005B - A kind of step carbonation high-quantum efficiency carbon quantum dot and preparation method thereof - Google Patents
A kind of step carbonation high-quantum efficiency carbon quantum dot and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of step carbonation high-quantum efficiency carbon quantum dot, purification, the preparation of phenylenediamine-citric acid nucleocapsid carbon quantum dot and the purification of phenylenediamine-citric acid nucleocapsid carbon quantum dot of preparation, carbon core including phenylenediamine carbon core.It is the cross-application of fluorescent technique and nanotechnology, it is first carbonized by phenylenediamine and forms carbon core, the reaction process of the secondary carbonization of citric acid is used again, and the nucleocapsid carbon dots synthesized by way of thermal cracking and carbonization have the characteristics that stability is good, biocompatibility is high, fluorescence efficiency is high.
Description
Technical field
The present invention is the preparation and application of biomaterial, is specifically obtained as raw material through step carbonation using phenylenediamine with citric acid
It is the cross-application of materialogy technology and fluorescent technique to the preparation method of fluorography material.
Background technique
It detects in medicine, fluorescent decoration object and determinand is chemically reacted into covalent bonding, make test substance by purple
Be changed into when excitation state is then restored to ground state when outer light or blue violet light are irradiated by ground state and issue fluorescence, via fluorescence microscope,
The purpose of instruments such as laser confocal microscope, flow cytometer detect, and can reach positioning, tracer, assay.This fluorescence
Labelling technique is component part important in molecular image technology, biochemistry, immunology, molecular biology, pathology and
Diagnostics etc. has obtained extensive utilization, greatly pushes such as early diagnosis of cancer, drug delivery, pathogen detection, induction
Stem cell therapy, the development of the emerging medical technology such as image guided surgery.With the development of science and technology, being made in fluorescent labelling techniques
There is emerging nano-luminescent material other than traditional organic fluorescence chemical substance in fluorescent material.Nano fluorescent material
Material has its distinctive advantage compared to traditional chemical fluorescent material：Its higher brightness and photostability, have more excellent
Solvent-dispersible and biocompatibility；Its nanoscale accurately controls and particle functionalization means become better and approaching perfection day by day, fluorescence emission
Spectrum is realized controllable to a certain extent, while ensuring exciting light spectrum width and continuous；Its nanoscale has large surface area, with it
Chemical group on its molecule forms covalent bond, and the substances such as connection protein, DNA realize modified and functionalization.Nanometer is glimmering
Luminescent material type is many, and carbon nanomaterial has size fluorescence associated property [1], is widely used in nano-luminescent material neck
Domain, including：Graphene [2], carbon nanotube [3], fullerene etc. have sp2The carbon material of structure.Carbon-based quanta point material due to
Hypotoxicity and high-quantum efficiency are got the attention in recent years, a variety of different organic matters such as glucose, citric acid, folic acid
[4] etc. it all can be used as raw material preparation carbon quantum dot.In addition, preparation method is also varied, it is broadly divided into two classes：Method from top to bottom
Method from bottom to top, including：Electrochemical synthesis [5], hydro-thermal/acidic oxidation method [6], microwave method [7], ultrasonic method [8], laser
Ablation and plasma processing method etc..In research before, scientific workers have found to utilize surface passivation, element
The different method such as doping and surface functionalization can effectively improve the quantum efficiency [9] of carbon quantum dot.
Summary of the invention
In order to overcome the deficiencies of the prior art, present invention aims at provide a kind of step carbonation high-quantum efficiency carbon quantum
The preparation method of point.Using phenylenediamine and citric acid as carbon source, gradation step carbonation prepares high-quantum efficiency carbon quantum dot material
Novel method.
Another object of the present invention is：A kind of step carbonation high-quantum efficiency carbon amounts that the preparation method obtains is provided
Sub- point.
A kind of preparation method of step carbonation high-quantum efficiency carbon quantum dot, which is characterized in that include the following steps：
（1）The preparation of phenylenediamine carbon core：
It include that o-phenylenediamine, m-phenylene diamine (MPD) and p-phenylenediamine are added in the ratio of 10mg/ml respectively by different structure phenylenediamine
Enter in dehydrated alcohol, be protected from light stirring at room temperature, until obtain uniform ethyl alcohol-phenylenediamine solution, respectively obtain it is colourless,
The solution of dusty blue, lightpink；Solution is placed in tetrafluoroethene hydrothermal reaction kettle, liquor capacity is no more than the 2/3 of reaction kettle,
180 DEG C of standings of high temperature react 6h in confined conditions；It after reacting sufficiently, is slowly cooled to room temperature, finally obtains yellow, greyish black
The phenylenediamine carbon quantum dot ethanol solution of color and reddish black；
（2）The purification of carbon core：
The carbon quantum dot ethanol solution of different phenylenediamines is placed in revolving instrument, under certain temperature revolving to ethyl alcohol and
Water volatilizees completely, obtains phenylenediamine carbon quantum dot crude product, chromatography solution is added into obtained oily thick liquid, stirring is extremely
Oily liquids is dispersed among solvent system, and acquired solution is slowly transferred among silica gel column chromatography, is stood and is waited carbon
Quantum dot crude product determines carbon dots layer position since solution polarity is gradually layered, by ultraviolet light detection, and acquires carbon dots
Solution, it is after to be collected, obtained carbon quantum dot organic solution is organic by the method removal chromatography therein of revolving
Acquired solution is freeze-dried by solvent then to pure water is added in obtained solid product, the phenylenediamine carbon needed for obtaining to the end
Core；
（3）The preparation of phenylenediamine-citric acid nucleocapsid carbon quantum dot：
By（2）Quantum dot obtained in step is dissolved in ethanol solution by 1mg/ml concentration, is added under conditions of being protected from light
1:1 1mg/ml citric acid solution is stirred until homogeneous, and obtains yellow, colourless and red solution, and solution is placed in tetrafluoroethene water
In thermal response kettle, liquor capacity is no more than the 2/3 of reaction kettle, and 180 DEG C of standings of high temperature react 6h in confined conditions；It is filled wait react
After point, it is slowly cooled to room temperature, finally obtains yellow, faint yellow and brown phenylenediamine-citric acid nucleocapsid carbon quantum dot solution；
（4）The purification of phenylenediamine-citric acid nucleocapsid carbon quantum dot：
Different phenylenediamines-citric acid nucleocapsid carbon quantum dot ethanol solution is placed in revolving instrument, in certain temperature backspin
Steaming is volatilized completely to ethyl alcohol and water, obtains carbon quantum dot crude product, and chromatography solution is added into obtained oily thick liquid, stirs
It mixes to oily liquids and is dispersed among solvent system, acquired solution is slowly transferred among silica gel column chromatography, stand carbon
Quantum dot crude product is gradually layered, and determines carbon dots layer position by ultraviolet light detection, and acquire carbon dots solution, to be collected complete
Obtained carbon quantum dot organic solution is removed chromatography organic solvent therein by the method for revolving, then to institute by Bi Hou
It obtains in solid product and pure water is added, acquired solution is freeze-dried, phenylenediamine-citric acid nucleocapsid carbon quantum dot is obtained.
A kind of step carbonation high-quantum efficiency carbon quantum dot, which is characterized in that be prepared according to the above method；With good
Good dissolving performance and optical stability, quantum efficiency reaches 40% ~ 60%, while having good biocompatibility, cell survival
Rate is greater than 80%.
The fluorescence quantum yield of carbon quantum dot provided by the invention is using conventional reference method measurement, i.e., in identical excitation item
Under part, fluorescence sample to be measured, the integrated fluorescence intensities of reference fluorescent standard substance of known quantum yield and same are measured respectively
The trap of the incident light of excitation wavelength, then by these values for people's following equation：
Wherein, Q and QRThe respectively fluorescence quantum yield of test substance and reference material；I and IRRespectively test substance and
The Fluorescence integral intensity of reference material；A and ARFor test substance and reference material the incident light of the excitation wavelength trap；
η and ηRThe respectively refractive index of sample to be tested and standard sample.It is provided by the invention after measured using quinine sulfate as reference substance
Carbon quantum dot fluorescence is 40% ~ 60%.
Present invention solves the technical problem that be that development carbon quantum dot is synthetically prepared problem, providing a kind of has stability
It is low to improve former carbon dots fluorescence efficiency to preparation method good, biocompatibility is high, fluorescence efficiency is high by gradation step carbonation
Problem, simple process, at low cost, easy repetition.
Present invention solves the technical problem that being the synthesis and preparation process problem of development carbon quantum dot, pass through gradation substep carbon
The method of change provides a kind of with the carbon quantum dot material preparation side that optical stability is good, biocompatibility is high, fluorescence efficiency is high
Method, simple process, easily repeat material high conversion rate.
The present invention has following advantage：
1, phenylenediamine carbon core multi-step carbonization enables the carburizing reagent of citric acid to be more easier completely, to improve the energy
Utilization efficiency, obtain higher quantum dot yield.
2, this method is carbon quantum dot raw material using phenylenediamine and citric acid, and raw material is simple and easy to get, using hydro-thermal method as high temperature
Carbonization method prepares water-soluble carbon dots fluorescent material, easy to operate, is easy to be commercialized.
3, the carbon dots biocompatibility of step carbonation preparation is good, can be applied to cell and histofluorescence imaging.
Detailed description of the invention
Fig. 1 is the preparation method process of embodiment.
Fig. 2 is the TEM photo that embodiment prepares gained carbon quantum dot.
Fig. 3 is the fluorescence spectrum of carbon quantum dot in embodiment 1.
Fig. 4 is the fluorescence spectrum of carbon quantum dot in embodiment 2.
Fig. 5 is the fluorescence spectrum of carbon quantum dot in embodiment 3.
Fig. 6 is the resulting HEK293 human embryonic kidney cells of carbon quantum dot development and U87mg brain glioblastoma cell laser co-focusing
Photo.
Fig. 7 is the HEK293 human embryonic kidney cells and U87mg brain glioblastoma cell toxicity profile of carbon quantum dot.
Specific embodiment
Fig. 1 is the preparation method process of embodiment.The preparation process of the hud typed carbon dots of phenylenediamine-citric acid such as attached drawing institute
Show, below by way of specific embodiment, the technical scheme of the present invention will be further described.Embodiment below is to the present invention
Further explanation, and do not limit the scope of the invention.
Embodiment 1：
O-phenylenediamine 0.1g is dissolved in be protected from light in 10ml ethyl alcohol and is stirred under room temperature, until phenylenediamine solid all dissolves,
Obtain uniform solution；It is placed in 50ml tetrafluoroethene reaction kettle and is placed in 6 hours of placement in 180 degrees Celsius of baking ovens.It is cooled to
After room temperature, acquired solution is removed into excess of solvent in 45 degrees Celsius of revolvings, methanol and dichloro are added into obtained oily liquids
The mixed solvent of methane stirs evenly, and settle and separate in silicagel column is slowly added dropwise in obtained solution, true by ultraviolet lamp
Determine carbon dots position, the carbon dots solution collected rotates carbon dots solution again, and after removing organic solvent therein, nothing is added
Water-ethanol to get arrive 10mg/ml phenylenediamine carbon quantum dot solution.0.1g citric acid is dissolved in 10ml pure water, is stirred at room temperature
It mixes, until citric acid is completely dissolved, phenylenediamine carbon dots solution and citric acid solution is mixed, 50ml tetrafluoroethene reaction kettle is placed in
In be placed in 180 degrees Celsius of baking ovens 6 hours of placement.After being cooled to room temperature, acquired solution is rotated in 45 DEG C, to obtained oil
Methanol is added in shape liquid and the mixed solvent of methylene chloride stirs evenly, obtained solution is slowly added dropwise in silicagel column
Settle and separate determines obtained carbon dots position by ultraviolet lamp, collects obtained carbon dots solution, the carbon dots solution that will be obtained
It rotates again, after removing organic solvent therein, dehydrated alcohol is added to get molten to phenylenediamine-citric acid nucleocapsid carbon quantum dot
Liquid.Fig. 2 is the TEM photo that embodiment prepares gained carbon quantum dot, and the carbon quantum dot Dispersed precipitate of preparation, size is in 5-
10nm range.Fig. 3 is the fluorescence spectrum of carbon quantum dot in embodiment 1：
Embodiment 2：
O-phenylenediamine 0.1g is dissolved in be protected from light in 10ml ethyl alcohol and is stirred under room temperature, until phenylenediamine solid all dissolves,
Obtain uniform solution；It is placed in 50ml tetrafluoroethene reaction kettle and is placed in 6 hours of placement in 180 degrees Celsius of baking ovens.It is cooled to
After room temperature, acquired solution is rotated in 45 DEG C, methanol is added into obtained oily liquids and the mixed solvent of methylene chloride stirs
It mixes uniformly, settle and separate in silicagel column is slowly added dropwise in obtained solution, obtained carbon dots position is determined by ultraviolet lamp
It sets, collects obtained carbon dots solution, obtained carbon dots solution is rotated again, after removing organic solvent therein, nothing is added
Water-ethanol to get arrive 10mg/ml phenylenediamine carbon quantum dot solution.0.1g citric acid is dissolved in 10ml pure water, is stirred at room temperature
It mixes, until citric acid is completely dissolved, phenylenediamine carbon dots solution and citric acid solution is mixed, 50ml tetrafluoroethene reaction kettle is placed in
In be placed in 180 degrees Celsius of baking ovens 6 hours of placement.After being cooled to room temperature, acquired solution is rotated in 45 DEG C, to obtained oil
Methanol is added in shape liquid and the mixed solvent of methylene chloride stirs evenly, obtained solution is slowly added dropwise in silicagel column
Settle and separate determines carbon dots position by ultraviolet lamp, collects obtained carbon dots solution, obtained carbon dots solution is revolved again
It steams, after removing organic solvent therein, dehydrated alcohol is added to get phenylenediamine-citric acid nucleocapsid carbon quantum dot solution is arrived.Fig. 4
For the fluorescence spectrum of carbon quantum dot in embodiment 2.
Embodiment 3：
P-phenylenediamine 0.1g is dissolved in be protected from light in 10ml ethyl alcohol and is stirred under room temperature, until phenylenediamine solid all dissolves,
Obtain uniform solution；It is placed in 50ml tetrafluoroethene reaction kettle and is placed in 6 hours of placement in 180 degrees Celsius of baking ovens.It is cooled to
After room temperature, acquired solution is rotated in 45 DEG C, methanol is added into obtained oily liquids and the mixed solvent of methylene chloride stirs
It mixes uniformly, settle and separate in silicagel column is slowly added dropwise in obtained solution, obtained carbon dots position is determined by ultraviolet lamp
It sets, collects obtained carbon dots solution, obtained carbon dots solution is rotated again, after removing organic solvent therein, nothing is added
Water-ethanol to get arrive 10mg/ml phenylenediamine carbon quantum dot solution.0.1g citric acid is dissolved in 10ml pure water, is stirred at room temperature
It mixes, until citric acid is completely dissolved, phenylenediamine carbon dots solution and citric acid solution is mixed, 50ml tetrafluoroethene reaction kettle is placed in
In be placed in 180 degrees Celsius of baking ovens 6 hours of placement.After being cooled to room temperature, acquired solution is rotated in 45 DEG C, to obtained oil
Methanol is added in shape liquid and the mixed solvent of methylene chloride stirs evenly, obtained solution is slowly added dropwise in silicagel column
Settle and separate determines obtained carbon dots position by ultraviolet lamp, collects obtained carbon dots solution, the carbon dots solution that will be obtained
It rotates again, after removing organic solvent therein, dehydrated alcohol is added to get molten to phenylenediamine-citric acid nucleocapsid carbon quantum dot
Liquid.Fig. 5 is the fluorescence spectrum of carbon quantum dot in embodiment 3.
The fluorescence property of carbon quantum dot nanoparticle is investigated：Carbon quantum dot obtained in embodiment 1 to 3 is placed in light splitting ware
In.Changing excitation wavelength respectively examines fluorescence exciting wavelength Detection wavelength from 300nm to 520nm, and the excitation wavelength detected is
450nm to 544nm, as shown in Fig. 3 to 5.It can be seen that three kinds of phenylenediamines-citric acid carbon quantum dot is excited in 380nm wavelength
When, strongest fluorescence exciting wavelength is 430nm.
Cell observes the development that carbon quantum dot nanoparticle swallows：
By HEK293 and U87mg cell, with 2 × 104The concentration of a cells/well is inoculated in (every hole in flat four points of wares
100 μ L train base), the carbon quantum dot material that 10 μ L various concentrations are added is mixed into serum training base in 37 DEG C, 5% CO2Item
It is incubated for 2 hours under part；Paraformaldehyde progress cell is added after being incubated for altogether to fix；Attached drawing 6 is that carbon quantum dot development is resulting
HEK293 human embryonic kidney cells and U87mg brain glioblastoma cell laser co-focusing photo.
The evaluation of carbon quantum dot cytotoxicity：Carbon quantum dot is prepared referring to the step of embodiment 1,2,3.To investigate its life
Object compatibility chooses HEK293 and U87mg cell, respectively with 2 × 104The concentration of a cells/well is inoculated in the training of 96 hole cells
It supports in plate (every 100 μ L of hole train base), the drug material of 10 μ L various concentrations is added, 37 DEG C in anteserum-less substrate, 5%
CO2Under the conditions of be incubated for 32 hours；75 μ L free serum culture based sols remove after being incubated for altogether, and supplement contains the fresh training of 10% serum
Base continues to cultivate 4h to 100 μ L；10 μ L Cell Counting Kit mono-Solution Cell Proliferation detection kit of Promega companies, which are added, to be incubated for
4h ；Data are read directly at microplate reader 490nm, calculate survival rate of the cell under various concentration effect.Fig. 7 is carbon quantum
The HEK293 human embryonic kidney cells and U87mg brain glioblastoma cell toxicity profile of point, it is seen then that carbon quantum dot is in 10~50mg/mL
Concentration range in HEK293 and U87mg cell influence.As carbon quantum concentration increases, the survival rate of cell is slightly in that decline becomes
Gesture, HEK293 and U87mg cell survival rate is 86.8% and 94.7% after 32 hours.
Claims (1)
1. a kind of preparation method of step carbonation high-quantum efficiency carbon quantum dot, which is characterized in that include the following steps：
（1）The preparation of phenylenediamine carbon core：
It include that nothing is added in the ratio of 10mg/ml respectively in o-phenylenediamine, m-phenylene diamine (MPD) and p-phenylenediamine by different structure phenylenediamine
In water-ethanol, it is protected from light stirring at room temperature, until obtaining uniform ethyl alcohol-phenylenediamine solution, respectively obtains colourless, grey indigo plant
The solution of color, lightpink；Solution is placed in tetrafluoroethene hydrothermal reaction kettle, liquor capacity is no more than the 2/3 of reaction kettle, close
180 DEG C of standings of high temperature react 6h under the conditions of closing；Wait react sufficiently after, be slowly cooled to room temperature, finally obtain yellow, grey black and
The phenylenediamine carbon quantum dot ethanol solution of reddish black, step carbonation high-quantum efficiency carbon quantum dot have excellent dissolution performance and
Optical stability, quantum efficiency reaches 40% ~ 60%, while having good biocompatibility, and cell survival rate is greater than 80%；
（2）The purification of carbon core：
The carbon quantum dot ethanol solution of different phenylenediamines is placed in revolving instrument, is rotated under certain temperature complete to ethyl alcohol and water
Full volatilization, obtains phenylenediamine carbon quantum dot crude product, and chromatography solution, stirring to oily are added into obtained oily thick liquid
Liquid is dispersed among solvent system, and acquired solution is slowly transferred among silica gel column chromatography, is stood and is waited carbon quantum
Point crude product determines carbon dots layer position by ultraviolet light detection, and acquire carbon dots solution since solution polarity is gradually layered,
After to be collected, obtained carbon quantum dot organic solution is removed into chromatography organic solvent therein by the method for revolving,
Then to pure water is added in obtained solid product, acquired solution is freeze-dried, the phenylenediamine carbon core needed for obtaining to the end；
（3）The preparation of phenylenediamine-citric acid nucleocapsid carbon quantum dot：
By（2）Quantum dot obtained in step is dissolved in ethanol solution by 1mg/ml concentration, and 1 is added under conditions of being protected from light:1
1mg/ml citric acid solution is stirred until homogeneous, and obtains yellow, colourless and red solution, and solution is placed in tetrafluoroethene hydro-thermal reaction
In kettle, liquor capacity is no more than the 2/3 of reaction kettle, and 180 DEG C of standings of high temperature react 6h in confined conditions；After reacting sufficiently,
It is slowly cooled to room temperature, finally obtains yellow, faint yellow and brown phenylenediamine-citric acid nucleocapsid carbon quantum dot solution；
（4）The purification of phenylenediamine-citric acid nucleocapsid carbon quantum dot：
By different phenylenediamines-citric acid nucleocapsid carbon quantum dot ethanol solution be placed in revolving instrument in, rotated under certain temperature to
Ethyl alcohol and water volatilize completely, obtain carbon quantum dot crude product, chromatography solution are added into obtained oily thick liquid, stirring is extremely
Oily liquids is dispersed among solvent system, and acquired solution is slowly transferred among silica gel column chromatography, stands carbon quantum
Point crude product is gradually layered, and determines carbon dots layer position by ultraviolet light detection, and acquire carbon dots solution, to be collected to finish
Afterwards, obtained carbon quantum dot organic solution is removed into chromatography organic solvent therein by the method for revolving, then to gained
Pure water is added in solid product, acquired solution is freeze-dried, obtains phenylenediamine-citric acid nucleocapsid carbon quantum dot.
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| CN106995699B (en) * | 2017-05-31 | 2018-06-01 | 中国矿业大学 | Carbon quantum dot prepared by the method and this method of the adjustable fluorescent carbon point of a large amount of synthetic wavelengths |
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| CN111592881B (en) * | 2020-05-29 | 2022-10-11 | 四川大学 | Carbon quantum dot capable of rapidly marking cell nucleus and preparation method and application thereof |
| CN111591979B (en) * | 2020-06-07 | 2023-04-21 | 西南大学 | Preparation method of single-layer graphene quantum dot with good photodynamic property |
| CN113443616B (en) * | 2021-07-06 | 2024-02-06 | 徐州工程学院 | Synthesis method of carbon quantum dot, carbon quantum dot and detection of Ag + Is a method of (2) |
| CN114213345A (en) * | 2021-12-23 | 2022-03-22 | 郑州中科生物医学工程技术研究院 | Method for separating yellow fluorescent substance from carbon quantum dots |
| CN114213344A (en) * | 2021-12-23 | 2022-03-22 | 郑州中科生物医学工程技术研究院 | Method for separating 2, 3-diaminophenazine from carbon quantum dots |
| CN115368891B (en) * | 2022-08-05 | 2023-10-24 | 扬州大学 | Fluorescent carbon quantum dot and application thereof in rapid chlorogenic acid detection |
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| CN105295909A (en) * | 2015-10-30 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for using phenylenediamine and citric acid for preparing carbon quantum dot marking probe for cell developing |
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