CN105567228A - N, P and S-codoped fluorescent carbon quantum dot and preparation method and application thereof - Google Patents
N, P and S-codoped fluorescent carbon quantum dot and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an N, P and S-codoped fluorescent carbon quantum dot and a preparation method and application thereof, and belongs to the technical field of luminescent nanomaterials. The preparation method comprises the steps that a biological bacterium (saccharomycete or escherichia coli or staphylococcus aureus or aspergillus niger) is taken as a carbon source, water of the corresponding volume is added, and a hydrothermal reaction is performed to obtain a dark brown solution; after the reaction stops and a reaction kettle is naturally cooled, dialysis is performed to remove impurities, an aqueous carbon quantum dot solution is obtained, and after freeze drying is performed, the N, P and S-codoped fluorescent carbon quantum dot is obtained. According to the method, the biomass is taken as the carbon source, the raw material is wide in source, low in cost, green and environmentally friendly, the technology is simple, and the preparation condition requirement is low. The obtained carbon quantum dot can be applied to detection on Cr (VI) ions, MnO4<-> and ascorbic acid by serving as a switch-type fluorescent probe and also can be used for cell imaging.
Description
Technical field
The present invention relates to Illuminant nanometer material, particularly relate to carbon quantum dot, the carbon quantum dot of a kind of N, P, the S codoped specifically utilizing biological mushroom to prepare and detect Cr (VI) ion, MnO as fluorescent probe
4 -and xitix etc., and the application in cell imaging.
Background technology
Quantum dot has superior optics due to it and electrical properties is subject to paying close attention to greatly and studying widely, it has the superior character such as quantum confined effect, surface effects, dimensional effect as accurate zero dimensional nanometer materials, and therefore quantum dot obtains good application in optics, electricity device, bio-imaging, biological medicine carrying etc.That traditional quantum dot research is more is semiconductor-quantum-point (such as CdSe, PbTe, CdTe etc.), it has shown huge potentiality in the application of biomedical sector especially in the dynamic tracer of cell, live body and imaging, but the introducing due to heavy metal element be its toxicity comparatively Datong District time have luminous unstable, easy flicker, and then limit its application on bio-imaging and biomarker, therefore finding desirable nontoxic nano level equivalent material becomes study hotspot.
Carbon quantum dot is a kind of novel nano material, is subject to the extensive concern of vast researcher in recent years.Carbon quantum dot refers to that size is less than the spherical nanoparticle of carbon of 10nm, and it has distinctive fluorescence excitation dependency.Compared with traditional semiconductor-quantum-point, it has the advantages such as good water solubility, high, the easy functionalization of chemical stability, resistance to photobleaching, low toxicity, good biocompatibility.These advantages make carbon quantum dot have broad application prospects in fields such as biology and medical science.
The preparation method of carbon quantum dot mainly contains two kinds at present, method (Top-down) and from bottom to top method (Bottom-up) from top to bottom.Top-to-bottom method mainly comprises arc-over, laser ablation, electrochemical oxidation, electron beam irradiation etc., and these class methods often need strict experiment condition or the special energy, and cost is high, and the fluorescence quantum yield of the carbon quantum dot obtained is lower; Bottom-to-top method mainly comprises combustion method, hydrothermal solution carborization, supports synthesis method, microwave method, supersonic method etc., but the raw material due to such method selection is all Nonrenewable energy resources and needs strict aftertreatment technology, so be also unfavorable for continuing and scale production carbon quantum dot.Therefore, find cheap and easy to get, aboundresources, Nantural non-toxic and environmentally friendly biological raw material as carbon source, the carbon quantum dot of preparation dopingization, high-fluorescence quantum yield is applied pharmaceutical analysis and cell imaging and is had great importance.Synthesize carbon quantum dot in a large number from the green carbon source of low cost under environmental protection prerequisite to be very important.Biomass are widespread in nature, cheap and easy to get, inexhaustible.Biomass are applied to the Green synthesis of nano material and the functional modification of some nanostructures, had both extended the Application Areas of biomass, and protected environment again, and therefore there is vast potential for future development.
Summary of the invention
The object of the present invention is to provide a kind of fluorescent carbon quantum dot of N, P, S codoped, and set up the preparation method of a kind of simple to operate, device simple, raw material environmental protection; And by described N, the carbon quantum dot of P, S codoped is used for ion, pharmaceutical analysis and cell imaging as fluorescent probe.
The preparation method of the carbon quantum dot of a kind of N, P, S codoped provided by the invention, comprises the following steps:
1) the biological mushroom powder of drying is joined in the water of certain volume, obtain the bacterium solution disperseed;
2) the bacterium solution obtained is transferred in hydrothermal reaction kettle, 4h-12h is reacted at 160 DEG C-240 DEG C, question response stops, after reactor naturally cooling, centrifugal segregation insolubles obtains the dark brown solution clarified, by the dialysis tubing of 500-1000Da, dialysis treatment at least 3 days in Glass Containers, namely pure N is obtained, the aqueous solution of the carbon quantum dot of P, S codoped;
3) target N is obtained by after the lyophilize of the above-mentioned carbon quantum dot aqueous solution, the carbon quantum dot of P, S codoped.
Step 1) described in biological mushroom be yeast, intestinal bacteria, streptococcus aureus or aspergillus niger.
Aforesaid method is with yeast or intestinal bacteria or streptococcus aureus, or aspergillus niger is carbon source, utilizes hydrothermal synthesis method, adulterates nitrogen phosphate and sulfur simultaneously in carbon quantum dot, obtains N, the carbon quantum dot of P, S codoped.
N prepared by aforesaid method, the carbon quantum dot of P, S codoped can be used as " switching mode " fluorescent probe for detecting Cr (VI) ion, MnO
4 -and xitix etc., also can be applicable to cell imaging.
Compared with prior art, the present invention has following beneficial effect:
(1) operation steps of the present invention is simple, does not need through surface passivator process or modifies the carbon quantum dot that can obtain nitrogen phosphorus sulphur codoped.
(2) biomass are widespread in nature, cheap and easy to get, inexhaustible.Starting material of the present invention only need biological mushroom, wide material sources, environmental protection, low price.
(3) the aim carbon quantum dot obtained by the present invention all has good solubleness and dispersiveness in aqueous.
(4) emission wavelength of aim carbon quantum dot itself red shift with the red shift of excitation wavelength.
(5) biological bacteria yeast-like fungi, streptococcus aureus, intestinal bacteria, aspergillus niger are as the microorganism extensively existed, and be applied in synthesis first, present method can expand to other microorganism simultaneously.
(6) quantum yield of aim carbon quantum dot is higher, and with Quinine Sulphate Di HC (quantum yield 54%) for object of reference, the quantum yield of gained carbon quantum dot is generally between 6.40%-12.68%.
In a word; operating procedure of the present invention is simple; raw material sources are extensive; environmental protection and low price, preparation condition requires low, and the carbon quantum dot optical property of gained nitrogen phosphorus sulphur codoped is stablized; fluorescence quantum yield is high; solving existing carbon quantum dot preparation method cannot large-scale production and obtain the lower problem of the fluorescence quantum efficiency of carbon quantum dot because technique and raw material restriction, and this carbon quantum dot can be applicable to Cr (VI) ion, MnO
4 -and the detection of xitix, and the field such as cell imaging.
Accompanying drawing explanation
Fig. 1 is N prepared by embodiment 1, the ultra-violet absorption spectrum of the carbon quantum dot of P, S codoped and fluorescent excitation-emmision spectra; Wherein fill the carbon quantum dot aqueous solution in quartz colorimetric utensil, be positioned on ultraviolet transmission platform, after 365nm excitation light source excites, send blue-fluorescence.
Fig. 2 is N prepared by embodiment 1, the spectrogram that the carbon quantum dot fluorescence emission curves of P, S codoped changes with excitation wavelength.
Fig. 3 is N prepared by embodiment 1, and the infrared spectrogram of the carbon quantum dot of P, S codoped, in figure, X-coordinate is determined wavelength, and ordinate zou is transmitance.
Fig. 4 is N prepared by embodiment 1, the XPS spectrum figure of the carbon quantum dot of P, S codoped.
Fig. 5 is N prepared by embodiment 1, the transmission electron microscope picture (left side) of the carbon quantum dot of P, S codoped and grain size distribution (right side).
Fig. 6 is the N of Cr (VI) cancellation embodiment 1 preparation, the fluorescence spectrum figure of the carbon quantum dot of P, S codoped.
Fig. 7 is N prepared by the embodiment 1 after xitix recovers Cr (VI) cancellation, the fluorescence spectrum figure of the carbon quantum dot of P, S codoped.
Fig. 8 is MnO
4 -n prepared by cancellation embodiment 1, the fluorescence spectrum figure of the carbon quantum dot of P, S codoped.
Fig. 9 is that xitix recovers MnO
4 -n prepared by the embodiment 1 after cancellation, the fluorescence spectrum figure of the carbon quantum dot of P, S codoped.
Figure 10 is N prepared by embodiment 1, the laser confocal imaging figure of the SiHa cell of the carbon quantum dot mark of P, S codoped;
Embodiment
Elaborate to the present invention below in conjunction with embodiment, embodiment gives detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the yeast taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 8h at 240 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 12.54%.
Fig. 1-10 is shown in property representation and application.
Embodiment 2
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the yeast taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 12h at 240 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 12%.
Embodiment 3
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the yeast taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 12h at 160 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 6.82%.
Embodiment 4
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the yeast taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 12h at 200 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 8.88%.
Embodiment 5
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the yeast taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 4h at 240 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 11.67%.
Embodiment 6
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the streptococcus aureus taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 8h at 240 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 12.68%.
Embodiment 7
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the intestinal bacteria taking 0.5g drying add in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 8h at 240 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 9.7%.
Embodiment 8
The preparation of the carbon quantum dot of N, P, S codoped:
Step 1, the aspergillus niger taking 0.5g drying adds in 10mL deionized water, the aqueous solution of obtained dispersion;
Step 2, transfers in hydrothermal reaction kettle by the mixed solution that step (1) obtains, hydro-thermal reaction 8h at 240 DEG C;
Step 3, product whizzer step (2) obtained with the centrifugal 10min of 6000r/min rotating speed, then is dialysed 3 days with the dialysis tubing that molecular weight cut-off is 500 ~ 1000Da, finally obtains N, the carbon quantum dot solution of P, S codoped.Its Relative quantum yields (taking Quinine Sulphate Di HC as standard) is 11.75%.
Embodiment 9
Quartz colorimetric utensil fills the N of embodiment 1, the fluorescent carbon quantum dot aqueous solution of P, S codoped, is positioned on ultraviolet transmission platform, after 365nm excitation light source excites, sends bright blue-fluorescence.
Embodiment 10
N prepared by embodiment 1, the carbon quantum dot aqueous solution fluorescence of P, S codoped can by Cr (VI) cancellation, and as shown in Figure 6, along with the increase of Cr (VI) ionic concn, the fluorescence intensity of carbon quantum dot reduces gradually.
Embodiment 11
N prepared by embodiment 1, P, the fluorescent carbon quantum dot aqueous solution of S codoped is recovered fluorescence by after Cr (VI) cancellation by xitix, as shown in Figure 7, along with the increase of ascorbic acid concentrations, the fluorescence intensity of carbon quantum dot is recovered gradually, and the carbon quantum dot prepared by explanation can be used as " switching mode " fluorescent probe.
Embodiment 12
N prepared by embodiment 1, the carbon quantum dot aqueous solution fluorescence of P, S codoped can by MnO
4 -cancellation, as shown in Figure 8, along with MnO
4 -the increase of ionic concn, the fluorescence intensity of carbon quantum dot reduces gradually.
Embodiment 13
N prepared by embodiment 1, the fluorescent carbon quantum dot aqueous solution of P, S codoped is by MnO
4 -recover fluorescence by xitix after cancellation, as shown in Figure 9, along with the increase of ascorbic acid concentrations, the fluorescence intensity of carbon quantum dot is recovered gradually, and the carbon quantum dot prepared by explanation can be used as " switching mode " fluorescent probe.
Embodiment 14
N prepared by embodiment 1, the carbon quantum dot aqueous solution (5mg/mL) of P, S codoped is for marking SiHa cell, and as shown in Figure 10, cellular form is good, and visual target carbon quantum dot does not have cytotoxicity, can be used for viable cell labelling.Figure 10 is from left to right followed successively by: details in a play not acted out on stage, but told through dialogues (exciting as 405nm) cytological map (blueness), details in a play not acted out on stage, but told through dialogues (exciting as 488nm) cytological map (green), blue and green stacking diagram.
Claims (8)
1. the preparation method of the fluorescent carbon quantum dot of a N, P, S codoped, is characterized in that, comprises the following steps:
1) the biological mushroom powder of drying is joined in the water of certain volume, obtain the bacterium solution disperseed;
2) the bacterium solution obtained is transferred in hydrothermal reaction kettle, 4h-12h is reacted at 160 DEG C-240 DEG C, question response stops, after reactor naturally cooling, centrifugal segregation insolubles obtains the dark brown solution clarified, by the dialysis tubing of 500-1000Da, dialysis treatment at least 3 days in Glass Containers, namely pure N is obtained, the aqueous solution of the carbon quantum dot of P, S codoped;
3) target N is obtained by after the lyophilize of the above-mentioned carbon quantum dot aqueous solution, the carbon quantum dot of P, S codoped.
2. the preparation method of the carbon quantum dot of a kind of N, P, S codoped as claimed in claim 1, is characterized in that step 2) described in hydrothermal temperature be 240 DEG C, reaction times 8h.
3. the preparation method of the carbon quantum dot of a kind of N, P, S codoped as claimed in claim 1, is characterized in that step 1) described in biological mushroom be yeast, intestinal bacteria, streptococcus aureus or aspergillus niger.
4. the N that as described in claim 1,2 or 3 prepared by method, the carbon quantum dot of P, S codoped.
5. the carbon quantum dot of N, P, S codoped as claimed in claim 4 is detecting the application in Cr (VI) ion.
6. the carbon quantum dot of N, P, S codoped as claimed in claim 4 is at detection MnO
4 -application in ion.
7. the carbon quantum dot of N, P, S codoped as claimed in claim 4 is detecting the application in xitix.
8. the application of carbon quantum dot in cell imaging of N, P, S codoped as claimed in claim 4.
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| CN106323931A (en) * | 2016-09-17 | 2017-01-11 | 湖南科技大学 | Method for quickly synthesizing carbon dots in microwave manner by using yeast bacteria as a main carbon source and using carbon dots to detect pH of solution |
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