CN107529514A - Adulterate the preparation method and applications of fluorine ion carbon point - Google Patents

Adulterate the preparation method and applications of fluorine ion carbon point Download PDF

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Publication number
CN107529514A
CN107529514A CN201710878666.0A CN201710878666A CN107529514A CN 107529514 A CN107529514 A CN 107529514A CN 201710878666 A CN201710878666 A CN 201710878666A CN 107529514 A CN107529514 A CN 107529514A
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China
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preparation
fluorine ion
carbon point
carbon
source
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CN201710878666.0A
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CN107529514B (en
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顾微
杨宛凝
彭信怡
叶玲
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Capital Medical University
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Capital Medical University
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Abstract

A kind of preparation method for adulterating fluorine ion carbon point, comprises the following steps:A) carbon source and nitrogen source are added into water;B) fluoride sources are added in step A solution;C microwave heating) is carried out to step B solution;D dialysed after) step C products therefroms are dissolved in water, obtain exciting in 520 550nm light and issue the doping fluorine ion carbon point of fluorescent red-orange.The preparation method of the present invention is simple and convenient, it is not necessary to which special consersion unit, cost are low.The carbon point of the present invention can be used for cell marking, and fluorescent red-orange is sent under excitation.

Description

Adulterate the preparation method and applications of fluorine ion carbon point
Technical field
The invention belongs to field of nano-luminescent material, and in particular to it is a kind of adulterate fluorine ion carbon point preparation method and its Using.
Background technology
Carbon point has good water solubility, small toxicity, fluorescence intensity height and stability as a kind of novel light-emitting nano material The advantages that good, it is a kind of preferably novel fluorescence marker material, there is important application value in biology and field of medicaments.
Carbon point prepared by existing " from bottom to top " method sends blueness under usual excitation or green is glimmering Light.And for the application in biological and medical field, particularly fluorescence imaging application, there is the orange red luminous of longer wavelength Carbon point shows bigger advantage because having smaller ambient interferences and stronger tissue penetration.At present, " by lower On " method prepare fluorescent red-orange carbon point mainly by hydro-thermal method, it is necessary to which longer generated time and special reaction are set It is standby.Ridge this, there is provided fluorescent red-orange carbon point prepared by a kind of simple and rapid method, for expanding carbon point in biology and medicine Further application is very important in field.
The content of the invention
In order to solve problems of the prior art, the invention provides a kind of preparation side for adulterating fluorine ion carbon point Method and its application.
On the one hand, the invention provides a kind of preparation method for adulterating fluorine ion carbon point, comprise the following steps:
A) carbon source and nitrogen source are added to the water;
B) fluoride sources are added in step A solution;
C) step B solution is heated;
D dialysed after) step C products therefroms are dissolved in water, obtain exciting in 520-550nm light and issue fluorescent red-orange The doped carbon point aqueous solution.
On the other hand, the invention provides a kind of doping fluorine ion carbon point prepared using the preparation method.
Another aspect, present invention also offers a kind of doping fluorine ion carbon point prepared using the preparation method thin Application in born of the same parents' mark, it comprises the following steps:
A) doping fluorine ion carbon point is incubated altogether with cell;
B) micro- sem observation cell marking situation is utilized.
Compared with prior art, technical scheme has the advantages that:
1) preparation method of the invention is simple and convenient, the reaction time is short, it is not necessary to special consersion unit, cost It is low;
2) carbon point of the invention sends fluorescent red-orange under excitation, has stronger penetration capacity, using model Enclose wider.
3) compared with no fluorine-ion-doped carbon point, it can make carbon point fluorescence that red shift occur after mixing fluorine ion.
Brief description of the drawings
Fig. 1 is the doping fluorine ion carbon point of the invention prepared the photo in the case where daylight and 530nm excite light irradiation respectively;
Fig. 2A is fluorescence hair of the doping fluorine ion carbon point of preparation of the embodiment of the present invention under different wave length excitation Spectrogram (a length of 520nm of excitation light wave to 550nm, step-length 10nm);
Fig. 2 B are the fluorescence undoped with fluorine ion carbon point under different wave length excitation prepared by comparative example of the present invention Luminous spectrogram (a length of 520nm of excitation light wave to 550nm, step-length 10nm);
Fig. 3 is the laser confocal microscope figure of doping fluorine ion carbon point marked tumor cell prepared by the present invention.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, and join According to accompanying drawing, the present invention is described in further detail.
The preparation method of doping fluorine ion carbon point of the present invention, comprises the following steps:
A) carbon source and nitrogen source are added to the water;
B) fluoride sources are added in step A solution;
C) step B solution is heated;
D dialysed after) step C products therefroms are dissolved in water, obtain exciting in 520-550nm light and issue fluorescent red-orange The doping fluorine ion carbon point aqueous solution.
One or more of the carbon source therein in citric acid, oxalic acid, ascorbic acid or its soluble-salt;Nitrogen source is selected One or more from urea, ethylenediamine or triethylamine;One or more of the fluoride sources in NaF, KF or NH4F.
The quality of carbon source and nitrogen source is 1: 1 to 1: 5 than scope, and the mass ratio of the two and water is 1: 10 to 1: 80, mixes fluorine The mass concentration of ion gun is 1-2%.
Step C) it is middle using microwave heating, the heat time is 3-5 minutes.
Step D) in dialysis dialysed using molecular cut off 100-500Da bag filter, dialysis time is preferably 12-24 hours.
The preparation method can also include:By the carbon point aqueous solution vacuum freeze drying in step D obtain adulterate fluorine from Sub- carbon point solid.
The invention further relates to application of the doping fluorine ion carbon point in cell marking, it comprises the following steps:
A) doping fluorine ion carbon point is incubated altogether with cell;
B) micro- sem observation cell marking situation is utilized.
Wherein described cell is tumour cell;The condition being incubated altogether is 37 DEG C, 5%CO2;The time being incubated altogether is 6-12 hours, the microscope can be laser confocal microscope or inverted fluorescence microscope.
Technical scheme is further illustrated with reference to specific embodiment.
Comparative example:
1) using 180mg citric acids as carbon source, 540mg urea is dissolved in 10ml water as nitrogen source;
2) using household microwave oven as thermal source, microwave heating 5 minutes is carried out to the solution of step 1;
3) products therefrom is obtained undoped with fluorine ion carbon water with molecular cut off 100Da bag filter dialysis purification Solution.
Embodiment one:
1) using 180mg citric acids as carbon source, 540mg urea is dissolved in 10ml water as nitrogen source;
2) 100mg sodium fluorides are mixed in the solution of step 1;
3) using household microwave oven as thermal source, microwave heating 5 minutes is carried out to the solution of step 2;
4) after products therefrom is dissolved in water with molecular cut off 100Da bag filter dialysis purification obtain adulterate fluorine from The sub- carbon point aqueous solution;
5) photoluminescent property of gained carbon point is characterized:With wavelength 530nm exciting light to adulterating fluorine ion carbon Point aqueous sample is irradiated, and obvious orange light (as shown in Figure 1) can be observed;Obtained with sepectrophotofluorometer different The fluorescence radiation spectrogram of carbon point under excitation wavelength (520-550nm, step-length 10nm), further confirm that the present invention is prepared and adulterate The luminous situation of fluorine ion carbon point (shown in Fig. 2A).(Fig. 2A and 2B compared with being prepared in comparative example undoped with fluorine ion carbon point It is shown), fluorine-ion-doped carbon point lights generation~5nm red shifts.
Embodiment two:
1) C6 glioma cells are inoculated in the 6 hole culture dishes for being placed with cover glass, in 37 DEG C, 5%CO2In incubator Culture;
2) after cell attachment, supernatant is sucked, the culture medium containing doping fluorine ion carbon point is added, in 37 DEG C, 5%CO2 It is incubated altogether in incubator 24 hours;
3) cover glass is taken out, is cleaned with PBS, fixed cell;
4) carbon point is observed under laser confocal microscope to C6 cell markings situation (as shown in Figure 3).
Particular embodiments described above, the purpose of the present invention, technical scheme and beneficial effect are carried out further in detail Describe in detail bright, it should be understood that the foregoing is only the present invention specific embodiment, be not intended to limit the invention, it is all Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., the protection of the present invention should be included in Within the scope of.

Claims (10)

1. a kind of preparation method for adulterating fluorine ion carbon point, comprises the following steps:
A) carbon source and nitrogen source are added to the water;
B) fluoride sources are added in step A solution;
C) step B solution is heated;
D dialysed after) step C products therefroms are dissolved in water, obtain exciting in 520-550nm light and issue the doping of fluorescent red-orange The fluorine ion carbon point aqueous solution.
2. preparation method according to claim 1, it is characterised in that:Carbon source therein is selected from citric acid, oxalic acid, Vitamin C One or more in acid or its soluble-salt;One or more of the nitrogen source in urea, ethylenediamine or triethylamine;Fluorine ion Source is selected from NaF, KF or NH4One or more in F.
3. preparation method according to claim 1, it is characterised in that:The quality of carbon source and nitrogen source is 1: 1 to 1 than scope: 5, the mass ratio of the two and water is 1: 10 to 1: 80, and the mass concentration for mixing fluoride sources is 1-2%.
4. preparation method according to claim 1, it is characterised in that:Step C) in heated using microwave, the heat time is 3-5 minutes.
5. preparation method according to claim 1, it is characterised in that:Step D) in dialysis utilize molecular cut off 100- 500Da bag filter is dialysed, and dialysis time is preferably 12-24 hours.
6. preparation method according to claim 1, it is characterised in that:The preparation method also includes:By the carbon in step D Point aqueous solution vacuum freeze drying obtains adulterating fluorine ion carbon point solid.
A kind of 7. doping fluorine ion carbon point prepared using preparation method any one of claim 1-6.
8. a kind of doping fluorine ion carbon point prepared using preparation method any one of claim 1-6 is in cell marking Application, it comprises the following steps:
A) doping fluorine ion carbon point is incubated altogether with cell;
B) micro- sem observation cell marking situation is utilized.
9. application as claimed in claim 8, it is characterised in that:The condition being incubated altogether is 37 DEG C, 5%CO2;It is incubated altogether Time is 6-12 hours, it is preferable that the cell is tumour cell.
10. application as claimed in claim 8, it is characterised in that:The microscope is laser confocal microscope or is inverted glimmering Light microscope.
CN201710878666.0A 2017-09-25 2017-09-25 Preparation method and application of fluorine ion-doped carbon dots Expired - Fee Related CN107529514B (en)

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CN110408389A (en) * 2019-08-05 2019-11-05 深圳大学 A kind of carbon quantum dot and its preparation method and application

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