CN106596874A - Carbon quantum dots in starch-based food and detection method and application of carbon quantum dots - Google Patents
Carbon quantum dots in starch-based food and detection method and application of carbon quantum dots Download PDFInfo
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- CN106596874A CN106596874A CN201710041955.5A CN201710041955A CN106596874A CN 106596874 A CN106596874 A CN 106596874A CN 201710041955 A CN201710041955 A CN 201710041955A CN 106596874 A CN106596874 A CN 106596874A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/10—Starch-containing substances, e.g. dough
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2004—Light-sensitive devices characterised by the electrolyte, e.g. comprising an organic electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
The invention provides carbon quantum dots in starch-based food and a detection method and application of the carbon quantum dots. The starch-based food is dried at low temperature, ground into powder, dissolved and separated to obtain clear liquid, and the carbon quantum dots in the starch-based food are accurately detected and evaluated by modes of ultraviolet light irradiation, an ultraviolet-visible light splitting spectrum, steady-state fluorescence spectrum, X-ray photoelectron spectroscopy, cyclic voltammetry, observation by a high-resolution transmission electron microscope and the like. Materials are taken from food materials closely linked to life, the carbon quantum dots which are in the starch-based food and affect health of human bodies are qualitatively and quantitatively detected by a simple and speedy method, the technology is accurate and speedy, a scientific basis is provided for safety detection of food of the human bodies, and the technology has guiding significance on a dietary mode of people. Meanwhile, the carbon quantum dots detected in the food are combined to a quantum dot sensitized solar cells, the cost is low, and pollution does not exist.
Description
Technical field
The invention belongs to the carbon quantum in nanometer technology and field of detection of food safety, more particularly to a kind of starch food products
Point and its detection method and application.
Background technology
Food-safety problem is always much-talked-about topic of concern.Wheat, as one of global three big cereal, is a kind of
In the grass extensively planted all over the world, wheat is worn into and can make after flour bread, steamed bun, biscuit, Pizza, noodles
Deng food.Rice is one of important cereal crops, and whole world population more than half is with rice as staple food.The shallow lake that the mankind are absorbed
Powder food is all that wheat or rice mix and obtained Jing after high-temperature heating with water.Contain various carbochain macromoleculars in starch,
There is hydrolysis in aqueous hot environment and generate glucose, glucose can generate carbon quantum dot again in this context.At present
There is experiment to confirm that large scale and the carbon quantum dot of high concentration there can be toxicity to zooblast and internal organ.As the master of human energy
Absorb source, how the security of evaluation starch based food and how the carbon quantum dot to wherein containing carries out quick, essence
Accurate detection is significant to human health.Meanwhile, carbon quantum dot unique properties are all in bio-sensing, photovoltaic device etc.
It is multi-field to be widely used.
The content of the invention
The invention provides the carbon quantum dot and its detection method and application in a kind of starch food products, the present invention adopts steamed bun
The conventional starch food such as head, bread, gruel, rice, Pizza, French fries, noodles, potato, it is complete retain food process technique and
It is dried in the case of COF, grinds, dissolves, is centrifuged, is subsequently tested and analyzed, testing result authenticity and reliability
Property it is high, detection method is simple, efficiently.Meanwhile, by the carbon quantum dot obtained in starch food products be used for prepare it is quantum dot sensitized too
Positive energy battery.
For achieving the above object, this experiment is employed the following technical solutions and is achieved：
The invention provides in a kind of starch food products carbon quantum dot detection method, it is comprised the following steps：
（1）Starch food products are put in drying box, powdery is ground to form after drying；
（2）Weigh above-mentioned starch food products powder to be dissolved in deionized water, ultrasound obtains suspension；
（3）By suspension centrifugation, solution to be measured is obtained；
（4）The solution to be measured is carried out into respectively following detection：It is positioned under uviol lamp and irradiates；Steady-state fluorescence spectrum test；It is purple
Outward-visible absorption spectra test；X-ray photoelectron spectroscopy is tested；High power transmission electron microscope observation；Cyclic voltammetric is surveyed
Examination, obtains the solution containing carbon quantum dot in starch food products.
Further：The step（1）The temperature of middle drying box is 50-70 DEG C, is dried 24 hours.
Further：The step（2）In the mass ratio of food powders and deionized water be 1:30-50, ultrasonic time 2
~ 4 hours.
Further：The step（4）Middle uviol lamp launch wavelength is 365nm, and luminous intensity is stronger, contains in food
Carbon quantum dot is more.
Further：The step（4）The test of middle steady-state fluorescence spectrum is：Respectively with 300nm-420nm, step-length is
The excitation wavelength of 20nm excites solution to be measured, the distinctive emission spectra Red Shift Phenomena of carbon quantum dot occurred in observation gained collection of illustrative plates.
Further：The step（4）Middle cyclic voltammetry is：Using standard three electrode system, platinum filament is used as to electricity
Solution to be measured is spin-coated on platinized platinum and is used as working electrode by pole, Ag/AgCl as reference electrode；Electrolyte is 0.1mol/L's
Tetrabutyl ammonium hexafluorophosphate.
Present invention also offers the solution containing carbon quantum dot in starch food products is preparing quantum dot sensitization solar electricity
Application in pond.
Further：The quantum dot sensitized solar cell is obtained by following steps：
(1) colloidal tio 2, is prepared, colloidal tio 2 is applied on FTO electro-conductive glass matrixes, high-temperature calcination prepares mesoporous
Titanium deoxid film,；
(2), light anode prepared by step (1) is immersed in the solution containing carbon quantum dot in starch food products, is made
The light anode of quantum dot solar cell；
(3), platinum is prepared to electrode using pyrolysismethod；
(4) platinum prepared by the light anode for, preparing step (2) and step (3) is to electrode assembling into quantum dot sensitized solar-electricity
Pond.
Further：The liquid electrolyte by 0.01～0.06 mol/L iodine, 0.08～0.12 mol/L lithium iodides,
The acetonitrile solution composition of 0.4～0.8 mol/L tetrabutylammonium iodides and 0.4～0.6 mol/L 4- tert .-butylpyridines.
Further：The open-circuit voltage of the quantum dot sensitized solar cell is 0.3～0.6V, short circuit current is 0.2
～0.7mA cm-2, photoelectric transformation efficiency be 0.1～0.3%.
The present invention mainly has the advantage that using after above technical scheme：
（1）Sample preparation is simple.The starch food that directly has drawn from of the invention, it is not necessary to which secondary operation, step is simple, it is convenient to promote.
（2）Detection is accurate.The present invention directly carries out low temperature drying to starch food, without the need for adding additional agents, tests sample
Product completely preserve the primary characteristic in food, as a result accurately.
（3）Experimental period is short.Sample low temperature drying can be drawn precise results by the present invention within 48 hours, be not required to
Loaded down with trivial details experimental arrangement is wanted, quickly and efficiently the carbon quantum dot in starch-containing food can be detected.
（4）The present invention can also be used for the carbon quantum dot obtained from starch food products preparing quantum dot sensitization solar electricity
Pond, expands the range of application of carbon quantum dot.
Description of the drawings
Fig. 1 be the present invention illumination wavelength is adopted in dark surrounds for 365nm ultra violet lamp bread core and crust
Solution, detects the luminescent effect of carbon quantum dot, wherein,（a）With（b）Difference corresponding surface cored and crust.
Fig. 2 is that the PL of the carbon quantum dot that the present invention is measured using steady-state fluorescence spectrometer opposite cored and crust solution swashs
Collection of illustrative plates is sent out, wherein,（a）With（b）Difference corresponding surface cored and crust.
Fig. 3 is the carbon quantum dot that the present invention is measured using ultraviolet-visible spectrophotometer opposite cored and crust solution
Uv-visible absorption spectra.
Fig. 4 is the present invention using x-ray photoelectron spectroscopy opposite cored and carbon quantum dot obtained in crust solution
X-ray photoelectron spectroscopy, wherein,（a）With（b）Difference corresponding surface cored and crust.
Fig. 5 is the present invention using high power transmission electron microscope opposite cored and the high power transmission plot of carbon quantum dot obtained in crust
Picture, wherein,（a）With（b）Difference corresponding surface cored and crust.
Fig. 6 is that the present invention is bent using the cyclic voltammetric of cyclic voltammetry opposite cored and carbon quantum dot obtained in crust
Line, wherein,（a）With（b）Difference corresponding surface cored and crust.
Fig. 7 is the present invention conventional starch food various to steamed bun, bread, gruel, rice, Pizza, French fries, noodles, potato etc.
Product adopt illumination wavelength for the ultra violet lamp of 365nm in dark surrounds, detect the luminescent effect of carbon quantum dot.
Fig. 8 is the carbon quantum dot extracted as carbon source with bread core of the invention J-V curves in the battery.
Specific embodiment
Technical scheme is further described with reference to specific embodiment.
Embodiment 1：
The detection method of carbon quantum dot specifically includes following steps in the present embodiment starch food products：
1st, laboratory sample is prepared using bread core：Obtained soft tommy core 10g is taken, baking oven is put into, after 60 DEG C are placed 24 hours,
Grind into powder；
2nd, 1g will be weighed with powder obtained in bread core, in being dissolved in the deionized water of 40ml, ultrasound obtains suspended for 2 ~ 4 hours
Liquid；
3rd, by above-mentioned solution centrifugal, centrifugal rotational speed is 5000-8000r/min, takes upper strata settled solution as solution to be measured；
4th, following detection is carried out respectively to the solution to be measured：It is positioned under uviol lamp and irradiates；Carry out steady-state fluorescence spectrum test；
Carry out uv-visible absorption spectra test；Carry out x-ray photoelectron spectroscopy test；Carry out high power transmission electron microscope sight
Examine；It is circulated volt-ampere test.
（1）, with ultra violet lamp solution to be measured.Solution 6ml to be measured is taken into vial, under dark surrounds transmitted wave is used
A length of 365mn ultra violet lamps solution to be measured, as shown in figure 1, sample sends blue light.Can be according to luminous strong and weak preliminary judgement
The content of carbon quantum dot in sample.Luminous intensity is stronger, and the carbon quantum dot contained in food is more.As shown in fig. 7, steamed bun, face
Various conventional starch foods such as bag, gruel, rice, Pizza, French fries, noodles, potato detect the luminescent effect of carbon quantum dot.
（2）, with XRF solution to be measured is tested.Solution 3ml to be measured is taken into four-way cuvette and is put into
In steady-state fluorescence spectrometer, respectively with 300nm-420nm, step-length excites sample, gained collection of illustrative plates for the different excitation wavelengths of 20nm
In there is the distinctive emission spectra Red Shift Phenomena of carbon quantum dot, from Fig. 2（a）In it can be seen that excite what sample was obtained with 340nm
Transmitting spectrum peak highest.
（3）, with ultraviolet-visible spectrophotometer solution to be measured is tested.Solution 3ml to be measured is taken to quartz colorimetric utensil
In and be put in ultraviolet-uisible spectrophotometer.Fig. 3 be by respectively with bread core and crust as raw material obtained in solution carry out
Test, as can be seen from the figure the strength ratio bread core of the ultraviolet absorption peak of crust obtained solution is strong, shows food containing flour
The content of middle diverse location carbon quantum dot is different.Ultraviolet absorption peak corresponds to the π → π of C=C in 280nm*.Further determine that
Contain carbon quantum dot in solution to be measured.
（4）, with x-ray photoelectron spectroscopy solution to be measured is tested.Solution to be measured is poured in culture dish and is put into
Baking oven, 60 DEG C of placements obtain powder to be measured in 24 hours.Powder to be measured is adopted into x-ray photoelectron spectroscopy, X-ray light is measured
Electron spectrum.From Fig. 4（a）As can be seen that containing C=C, C=O, C-O in solution to be measured.
（5）, with high power transmission electron microscope solution to be measured is tested.The high power of carbon quantum dot is detected in solution to be measured
Electron microscope.From high power Electronic Speculum Fig. 5（a）In clearly high power display carbon quantum dot can be surveyed using solution to be measured obtained in bread core
About 8 nanometers of diameter, can be used to intuitively to analyze whether the carbon quantum dot in food can produce injury to human body.
（6）, be circulated to carbon quantum dot volt-ampere test.Using standard three electrode system, platinum filament is used as to electrode, Ag/
Solution to be measured is spin-coated on platinized platinum and is used as working electrode by AgCl as reference electrode.Such as Fig. 6（a）, it can be seen from curve, Eox
=1.06 V, Ered=0.469V, HOMO=-5.46 V, the V of LUMO=- 3.85.
Embodiment 2：
The detection method of carbon quantum dot specifically includes following steps in the present embodiment starch food products：
1st, laboratory sample is prepared using crust：Obtained soft tommy skin 10g is taken, baking oven is put into, after 60 DEG C are placed 24 hours,
Grind into powder；
2nd, 1g will be weighed with raw material obtained in crust, in being dissolved in the deionized water of 40ml, ultrasound obtains suspended for 2 ~ 4 hours
Liquid；
3rd, by above-mentioned solution centrifugal, centrifugal rotational speed is 5000-8000r/min, takes upper strata settled solution as solution to be measured；
4th, following detection is carried out respectively to the solution to be measured：It is positioned under uviol lamp and irradiates；Carry out steady-state fluorescence spectrum test；
Carry out uv-visible absorption spectra test；Carry out x-ray photoelectron spectroscopy test；Carry out high power transmission electron microscope sight
Examine；It is circulated volt-ampere test.
（1）, with ultra violet lamp solution to be measured.Solution 6ml to be measured is taken into vial, under dark surrounds transmitted wave is used
A length of 365mn ultra violet lamps solution to be measured, as shown in figure 1, sample sends blue light.Can be according to luminous strong and weak preliminary judgement
The content of carbon quantum dot in crust sample.Luminous intensity is stronger, and the carbon quantum dot contained in food is more.
（2）, with XRF solution to be measured is tested.Solution 3ml to be measured is taken into four-way cuvette and is put into
In steady-state fluorescence spectrometer, respectively with 300nm-420nm, step-length excites sample, gained collection of illustrative plates for the different excitation wavelengths of 20nm
In there is the distinctive emission spectra Red Shift Phenomena of carbon quantum dot, and Fig. 2（b）In it can be seen that excite what sample was obtained with 360nm
Transmitting spectrum peak highest.
（3）, with ultraviolet-visible spectrophotometer solution to be measured is tested.Solution 3ml to be measured is taken to quartz colorimetric utensil
In and be put in ultraviolet-uisible spectrophotometer.Fig. 3 be by respectively with bread core and crust as raw material obtained in solution carry out
Test, as can be seen from the figure the strength ratio bread core of the ultraviolet absorption peak of crust obtained solution is strong, shows food containing flour
The content of middle diverse location carbon quantum dot is different.Ultraviolet absorption peak corresponds to the π → π of C=C in 280nm*.Further determine that
Contain carbon quantum dot in solution to be measured.
（4）, with x-ray photoelectron spectroscopy solution to be measured is tested.Solution to be measured is poured in culture dish and is put into
Baking oven, 60 DEG C of placements obtain powder to be measured in 24 hours.Powder to be measured is adopted into x-ray photoelectron spectroscopy, X-ray light is measured
Electron spectrum.From Fig. 4（b）Can draw, C=C, C=O, C-O are contained in solution to be measured.
（5）, with high power transmission electron microscope solution to be measured is tested.The high power of carbon quantum dot is detected in solution to be measured
Electron microscope.From high power Electronic Speculum Fig. 5（b）In clearly high power display carbon quantum dot can be surveyed using solution to be measured obtained in crust
About 16 nanometers of diameter, the carbon quantum dot diameter measured by the obvious specific surface cored system of crust is big.The result can be used to intuitively
Whether the carbon quantum dot in analysis food can produce injury to human body.
（6）, be circulated to carbon quantum dot volt-ampere test.Using standard three electrode system, platinum filament is used as to electrode, Ag/
Solution to be measured is spin-coated on platinized platinum and is used as working electrode by AgCl as reference electrode.Electrolyte is the tetrabutyl of 0.1mol/L
Ammonium hexafluorophosphate.Such as Fig. 6（b）, it can be seen from curve, Eox=0.95 0V, Ered=0.497V, HOMO=-5.225 V, LUMO
= -3.921 V。
Embodiment 3
The carbon quantum dot obtained in starch food products is used for the present embodiment the application of quantum dot sensitized solar cell（With bread
As a example by core）Specifically include following steps：
1st, colloidal tio 2 is prepared using sol-gel self-combustion synthesis, colloidal tio 2 is applied on FTO electro-conductive glass matrixes, Jing
400～500 DEG C of calcinings prepare mesoporous titanium dioxide film；
2nd, titanium deoxid film prepared by step 1 is immersed in extracting from bread core and is detected containing the molten of carbon quantum dot
In liquid, soak time is 20～30 hours；Make the light anode of quantum dot solar cell；
3rd, using pyrolysismethod platinum is prepared to electrode；
Platinum prepared by the light anode and step 3 for the 4, preparing step 2 adds liquid electrolyte assembling to electrode combination middle
Into quantum dot sensitized solar cell.
The liquid electrolyte by 0.01～0.06 mol/L iodine, 0.08～0.12 mol/L lithium iodides, 0.4～0.8
The acetonitrile solution composition of mol/L tetrabutylammonium iodides and 0.4～0.6 mol/L 4- tert .-butylpyridines.
As shown in figure 8, the obtained quantum dot sensitized solar cell open-circuit voltage of the present invention is 0.3～0.7V, it is short
Road electric current is 0.2～0.7mA cm-2, photoelectric transformation efficiency be 0.1～0.3%.
Above example is only illustrating technical scheme, rather than is limited；Although with reference to aforementioned reality
Apply example to be described in detail the present invention, for the person of ordinary skill of the art, still can be to aforementioned enforcement
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these are changed or replace
Change, do not make the spirit and scope of the essence disengaging claimed technical solution of the invention of appropriate technical solution.
Claims (10)
1. in a kind of starch food products carbon quantum dot detection method, it is characterised in that：It is comprised the following steps：
（1）Starch food products are put in drying box, powdery is ground to form after drying；
（2）Weigh above-mentioned starch food products powder to be dissolved in deionized water, ultrasound obtains suspension；
（3）By suspension centrifugation, solution to be measured is obtained；
（4）The solution to be measured is carried out into respectively following detection：It is positioned under uviol lamp and irradiates；Steady-state fluorescence spectrum test；It is purple
Outward-visible absorption spectra test；X-ray photoelectron spectroscopy is tested；High power transmission electron microscope observation；Cyclic voltammetric is surveyed
Examination, obtains the solution containing carbon quantum dot in starch food products.
2. in starch food products according to claim 1 carbon quantum dot detection method, it is characterised in that：The step
（1）The temperature of middle drying box is 50-70 DEG C, is dried 24 hours.
3. in starch food products according to claim 1 carbon quantum dot detection method, it is characterised in that：The step
（2）In the mass ratio of food powders and deionized water be 1:30-50, ultrasonic time 2 ~ 4 hours.
4. in starch food products according to claim 1 carbon quantum dot detection method, it is characterised in that：The step
（4）Middle uviol lamp launch wavelength is 365nm, and luminous intensity is stronger, and the carbon quantum dot contained in food is more.
5. in starch food products according to claim 1 carbon quantum dot detection method, it is characterised in that：The step
（4）The test of middle steady-state fluorescence spectrum is：300nm-420nm, step-length is used to excite solution to be measured for the excitation wavelength of 20nm respectively,
The distinctive emission spectra Red Shift Phenomena of carbon quantum dot occurred in observation gained collection of illustrative plates.
6. in starch food products according to claim 1 carbon quantum dot detection method, it is characterised in that：The step
（4）Middle cyclic voltammetry is：Using standard three electrode system, used as to electrode, Ag/AgCl, will used as reference electrode for platinum filament
Solution to be measured is spin-coated on platinized platinum and is used as working electrode；Electrolyte is the tetrabutyl ammonium hexafluorophosphate of 0.1mol/L.
7. the solution containing carbon quantum dot in starch food products that the detection method described in claim 1 is obtained is preparing quantum dot
Application in sensitization solar battery.
8. the solution containing carbon quantum dot in starch food products according to claim 7 is preparing quantum dot sensitization solar
Application in battery, it is characterised in that：The quantum dot sensitized solar cell is obtained by following steps：
(1) colloidal tio 2, is prepared, colloidal tio 2 is applied on FTO electro-conductive glass matrixes, high-temperature calcination prepares mesoporous
Titanium deoxid film,；
(2), light anode prepared by step (1) is immersed in the solution containing carbon quantum dot in starch food products, is made
The light anode of quantum dot solar cell；
(3), platinum is prepared to electrode using pyrolysismethod；
(4) platinum prepared by the light anode for, preparing step (2) and step (3) is to electrode assembling into quantum dot sensitized solar-electricity
Pond.
9. the solution containing carbon quantum dot in starch food products according to claim 8 is preparing quantum dot sensitization solar
Application in battery, it is characterised in that：The liquid electrolyte is by 0.01～0.06 mol/L iodine, 0.08～0.12 mol/L iodine
Change the acetonitrile solution composition of lithium, 0.4～0.8 mol/L tetrabutylammonium iodides and 0.4～0.6 mol/L 4- tert .-butylpyridines.
10. the solution containing carbon quantum dot in starch food products according to claim 8 is preparing the quantum dot sensitized sun
Application in energy battery, it is characterised in that：The open-circuit voltage of the quantum dot sensitized solar cell is 0.3～0.6V, short circuit
Electric current is 0.2～0.7mA cm-2, photoelectric transformation efficiency be 0.1～0.3%.
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