CN107955603A - A kind of water-solubility fluorescent carbon quantum dot and preparation method thereof and a kind of method for detecting fructose - Google Patents
A kind of water-solubility fluorescent carbon quantum dot and preparation method thereof and a kind of method for detecting fructose Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of water-solubility fluorescent carbon quantum dot, comprise the following steps：Inkfish juice is prepared into after powder and is mixed with water, hydro-thermal reaction is carried out in confined conditions, obtains water-solubility fluorescent carbon quantum dot.The present invention prepares carbon quantum dot using inkfish juice as raw material using one step hydro thermal method, detects fructose using fluorescence detection method, this method is simple and quick to provide new method for the detection of fructose, expands fructose detection platform.
Description
Technical field
The invention belongs to Novel Carbon Nanomaterials technical field, and in particular to a kind of water-solubility fluorescent carbon quantum dot and its system
Preparation Method and a kind of method for detecting fructose.
Background technology
Carbon quantum dot is using carbon as skeleton structure, and diameter is less than the spherical nano particle of 10nm, in 2004 by Xu etc.
(Xu X, R, Gu Y, et al.J Am Chem Soe, 2004,126 (40):12736-12737) carrying in single-walled carbon nanotube
Obtained first in pure procedure.Carbon quantum dot is because of its small-size effect, skin effect, the spy such as excitation wavelength is wide, launch wavelength is adjustable
Property, show good chemical stability (Bourlinos et al., 2008a, 2008b；Baker and Baker,2010；
Bourlinos et al.,2008a,2008b；Xu et al., 2004), the performance such as water solubility, hypotoxicity.It is set to be cured in biology
Learn with cell imaging (Cao et al., 2007；Yang et al., 2009), the field such as ion detection is widely used valency
Value.In recent years, as the fast development of carbon nanomaterial, carbon quantum dot are low by its fluorescent stability, biocompatibility, toxicity
Deng excellent properties, increasingly paid close attention to be subject to researchers, and constantly its application value in every respect of exploratory development.But mesh
The preparation method of preceding carbon quantum dot is complicated.
Fructose is a kind of monose, is the isomer of glucose, it is largely present in the juice of fruit with free state
In honey.Pure fructose is clear crystal, and fusing point is 103~105 DEG C, is not easy to crystallize, and is usually viscous liquid, readily soluble
Yu Shui, ethanol and ether.At present, fructose is widely used in food, medicine, health products production.The common detection side of fructose
Method is high performance liquid chromatography, ion-exchange chromatography, mass spectrography etc..But there is presently no examined using carbon quantum dot for fructose
The method of survey.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of water-solubility fluorescent carbon quantum dot and its preparation
Method and a kind of method for detecting fructose, the present invention prepare water-soluble fluorescent carbon using inkfish juice as raw material using one step hydro thermal method
Quantum dot, and the water-solubility fluorescent carbon quantum dot can be used for the detection of fructose, simple and fast, and the detection for expanding fructose is put down
Platform.
The present invention provides a kind of preparation method of water-solubility fluorescent carbon quantum dot, comprise the following steps：
Inkfish juice is prepared into after powder and is mixed with water, hydro-thermal reaction is carried out in confined conditions, obtains water soluble fluorescence
Carbon quantum dot.
Preferably, the method that the inkfish juice is prepared into powder is：
A) fresh ink anchovy sauce is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge, precipitated
Thing；
B) obtained sediment is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge；
C) repeat step B), the obtained sediment cleaned up is dried and ground, obtains powder.
Preferably, the mass volume ratio of the powder and water is 1g：(15~20) mL.
Preferably, the temperature of the hydro-thermal reaction is 120~180 DEG C, when the time of the hydro-thermal reaction is 1~24 small.
Preferably, after the hydro-thermal reaction, further include after the hydro-thermal reaction product is centrifuged, supernatant liquor is cold
It is lyophilized dry, obtain water-solubility fluorescent carbon quantum dot.
Present invention also offers the water-solubility fluorescent carbon quantum dot that a kind of above-mentioned preparation method is prepared, the water solubility
Fluorescent carbon quantum dot has blue-fluorescence under 365nm ultra violet lamps, and is produced respectively at 320nm and 390nm excitation wavelengths
Maximum emission peak.
Present invention also offers a kind of method for detecting fructose, comprise the following steps：
Using fluorescence spectrum, at 320nm, under the conditions of 3- amino phenyl boric acid (APBA) is existing, above-mentioned water solubility is utilized
Fructose in fluorescent carbon quantum dot detection sample to be tested.
Preferably, the sample to be tested is selected from honey.
Compared with prior art, the present invention provides a kind of preparation method of water-solubility fluorescent carbon quantum dot, including it is following
Step：Inkfish juice is prepared into after powder and is mixed with water, carries out hydro-thermal reaction in confined conditions, obtains water soluble fluorescence carbon amounts
Sub- point.The present invention prepares carbon quantum dot using inkfish juice as raw material using one step hydro thermal method, and fructose is detected using fluorescence detection method,
This method is simple and quick to provide new method for the detection of fructose, expands fructose detection platform.
Brief description of the drawings
Fig. 1 is the SEM figures of form of inkfish juice itself；
Fig. 2 is the TEM figures of water-solubility fluorescent carbon quantum dot prepared by embodiment 1；
Fig. 3 is the fluorescence spectra of water-solubility fluorescent carbon quantum dot prepared by embodiment 1；
Fig. 4 is water-solubility fluorescent carbon quantum dot aqueous solution photo (left side) under fluorescent light and in 365nm ultraviolet lightings
Photo (right side) under penetrating；
Fig. 5 is the selective enumeration method figure of the fructose of embodiment 2；
Fig. 6 is the influence figure that 3 glucose of embodiment detects fructose；
Fig. 7 is detected figure for embodiment 4 to different fructose concentrations.
Embodiment
The present invention provides a kind of preparation method of water-solubility fluorescent carbon quantum dot, comprise the following steps：
Inkfish juice is prepared into after powder and is mixed with water, hydro-thermal reaction is carried out in confined conditions, obtains water soluble fluorescence
Carbon quantum dot.
Inkfish juice is prepared into powder by the present invention first, and specific method is：
A) fresh ink anchovy sauce is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge, precipitated
Thing；
B) obtained sediment is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge；
C) repeat step B), the obtained sediment cleaned up is dried and ground, obtains powder.
The present invention prepares water-solubility fluorescent carbon quantum dot by raw material of fresh ink anchovy sauce, wherein, the fresh ink anchovy sauce choosing
Inkfish ink sac juice from Qingdao.
After fresh inkfish juice is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge, sunk
Starch.Wherein, the rotating speed of the centrifugation is 5000r/min, and the time of centrifugation is 20min.The volume ratio of the inkfish juice and water
Preferably 1mL:(3~5) mL, is preferably 1mL:(4~5) mL.
Then, obtained sediment is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge.Its
In, the rotating speed of the centrifugation is 5000r/min, and the time of centrifugation is 20min.The mass volume ratio of the sediment and water is preferred
For 1g：(20~30) mL, is preferably 1g：(24~26) mL.
The step of obtained sediment is mixed with water again, repeats to stand centrifugation.Wherein, the number of the repetition is preferably
1~4 time.Finally obtain the sediment cleaned up.
The sediment cleaned up is dried and ground, obtains powder.Wherein, the drying preferably in an oven into
Row drying, the temperature of the drying is preferably 40~60 DEG C, is preferably 50 DEG C.After sediment is dried, it is ground, obtains powder
End.
Then, obtained powder is mixed with water, carries out hydro-thermal reaction in confined conditions, obtain water soluble fluorescence carbon amounts
Sub- point.
Wherein, the mass volume ratio of the powder and water is preferably 1g：(15~20) mL.
After mixing, mixture is obtained, the mixture is placed in reaction kettle under conditions of closed and carries out hydro-thermal reaction.
Wherein, the reaction kettle is preferably ptfe autoclave.
The temperature of the hydro-thermal reaction is 120~180 DEG C, is preferably 140~160 DEG C, and the time of the hydro-thermal reaction is 1
~24 it is small when, be preferably 8~16 it is small when.
After the hydro-thermal reaction, further include after the hydro-thermal reaction product is centrifuged, supernatant liquor be freeze-dried,
Obtain water-solubility fluorescent carbon quantum dot.
The rotating speed of the centrifugation is preferably 8000r/min, and the time is preferably 15min.
Supernatant is obtained after centrifugation, the supernatant is freeze-dried, obtains water-solubility fluorescent carbon quantum dot.This hair
The bright specific method to the freeze-drying is not particularly limited, and well known to a person skilled in the art freeze-drying method.
After obtaining water-solubility fluorescent carbon quantum dot, the water-solubility fluorescent carbon quantum dot is kept in dark place in 4 DEG C of refrigerator
In.
Present invention also offers the water-solubility fluorescent carbon quantum dot that a kind of above-mentioned preparation method is prepared, the water solubility
Fluorescent carbon quantum dot has blue-fluorescence under 365nm ultra violet lamps, and is produced respectively at 320nm and 390nm excitation wavelengths
Maximum emission peak.
And have at 320nm and 390nm and respectively have a maximum excitation peak.
The water-solubility fluorescent carbon quantum dot is dissolved in the water, is colourless transparent liquid.
Present invention also offers a kind of method for detecting fructose, comprise the following steps：
Using fluorescence spectrum, at 320nm, under the conditions of APBA is existing, examined using above-mentioned water-solubility fluorescent carbon quantum dot
Survey the fructose in sample to be tested.
Specifically, after APBA, water-solubility fluorescent carbon quantum dot, testing sample solution and buffer solution are mixed, carry out
Fluorescence spectrum detects.The buffer solution is preferably PBS buffer solutions.
Wherein, testing principle is：Water-solubility fluorescent carbon quantum dot provided by the invention excitation wavelength 320nm excitation under,
When APBA is not present, fructose does not influence the fluorescence of carbon quantum；Carbon quantum dot Fluorescence Increasing after APBA is added, adds
Fluorescence intensity can be reduced again after fructose, fructose is detected with this.
If quantitative detection is carried out to the fructose in sample to be tested, it is preferred to use external standard method carries out the system of fructose standard curve
Make, be specially：
By the fructose aqueous solution of the standard sample of fructose configuration various concentrations, by with APBA and water soluble fluorescence carbon quantum
After point mixing, mixed solution is obtained, the mixed solution is detected by fluorescence spectrum, obtains different fluorescence intensities, so that
To fructose concentration and the standard curve of fluorescence intensity.
Preferably, the concentration of APBA is preferably 0.01~0.03mg/mL in the mixed solution, water soluble fluorescence carbon quantum
The concentration of point is preferably 0.05~0.07mg/mL, the concentration of fructose be respectively 33.33mM, 25mM, 16.67mM, 13.33mM,
8.33mM、5mM、4.17mM、3.33mM、2.5mM、1.67mM、1.33mM、1.00mM、0.67mM、l0.5mM、0.133mM、
0.1mM、0.083mM、0.05mM。
Fructose detection method provided by the invention, relative to glucose (G), mannose (S), galactolipin (Ga), xylose
(X), rhamnose (R), arabinose (A), L-fucose (L-F) and D- fucoses (D-F), sucrose, it is bright to the selectivity of fructose
It is aobvious.
Fructose detection method provided by the invention can be used for the qualitative and quantitative detection of fructose in the various materials containing fructose,
Wherein, test substance can be the food such as honey.
The present invention is prepared for a kind of water-solubility fluorescent carbon quantum dot, and the water-solubility fluorescent carbon quantum dot is using inkfish juice as raw material
Prepared using one step hydro thermal method, it is simple and convenient, without expensive instrument and equipment.The quantum dot prepared is water white transparency liquid
Body has good water solubility, stability.There is blue-fluorescence under 365nm ultra violet lamps, and excited in 320nm and 390nm
Maximum emission peak is produced at wavelength respectively.Biological imaging can be widely applied to according to the performance of the carbon quantum dot, material
Detection etc..The present invention is used for the detection of fructose with the water-solubility fluorescent carbon quantum dot of the synthesis, and of low cost, very simple is fast
Victory, expands the detection platform of fructose.
For a further understanding of the present invention, with reference to embodiment to water-solubility fluorescent carbon quantum dot provided by the invention and
The method of its preparation method and detection fructose illustrates, and protection scope of the present invention is not limited by the following examples.
APBA and fructose are that domestic analysis is pure in following embodiments, and wherein APBA concentration is 3mg/mL.
Embodiment 1
Preparation method using inkfish juice as the new carbon quantum dot of raw material：
1) 5000r/min centrifugations 20min takes heavy after the inkfish ink sac juice of Qingdao being added purified water soak at room temperature overnight
Form sediment, repeated washing 2 times, removes impurity.Clean after being dried in 50 DEG C of baking ovens and be ground into powder, treated in -20 DEG C of preservations
With.Wherein, electron microscopic observation, the result is shown in Figure 1 are scanned to fresh ink anchovy sauce, Fig. 1 is the SEM figures of form of inkfish juice itself.
2) by the raw material handled well in previous step in the liner of ptfe autoclave, 1g material powders are sequentially added
It is fitted into 15-20mL purified waters in reaction kettle.When reaction 24 is small in 180 DEG C of baking ovens.It is cooled to room temperature after reaction,
15min is centrifuged under 8000r/min and takes supernatant.It is kept in dark place after freeze-drying in 4 DEG C of refrigerators.
The above-mentioned water-solubility fluorescent carbon quantum dot being prepared is subjected to transmission electron microscope observation, the result is shown in Fig. 2, figure
The TEM figures of 2 water-solubility fluorescent carbon quantum dots prepared for embodiment 1.
The above-mentioned water-solubility fluorescent carbon quantum dot being prepared is subjected to fluorescence spectrum detection under the conditions of different wave length, is tied
Fruit sees that Fig. 3, Fig. 3 are the fluorescence spectra of water-solubility fluorescent carbon quantum dot prepared by embodiment 1.From the figure 3, it may be seen that in excitation wavelength
In the range of 260nm to 410nm, significant change occurs for the fluorescence intensity of the water-solubility fluorescent carbon quantum dot, illustrates the carbon quantum dot
Transmitting light has obvious excitation wavelength dependence, and produces emission maximum respectively at 320nm and 390nm excitation wavelengths
Peak.
The above-mentioned water-solubility fluorescent carbon quantum dot being prepared is dissolved in the water to obtain aqueous solution, the aqueous solution is existed
Have blue-fluorescence under 365nm ultra violet lamps, the result is shown in Fig. 4, Fig. 4 for water-solubility fluorescent carbon quantum dot aqueous solution under fluorescent light
Photo (left side) and the photo (right side) under 365nm ultraviolet lights.
Embodiment 2
1) 0.02mM is prepared, the PBS buffer solutions of pH=7.4, take 3mg APBA to be dissolved in 100mL PBS, obtain APBA's
PBS solution；
Glucose (G) 0.7206g, mannose (S) 0.7206g, galactolipin (Ga) 0.7206g, xylose (X) are weighed respectively
0.6005g, rhamnose (R) 0.7287g, fructose (Fr) 0.7206g, arabinose (A) 0.6006g, L-fucose (L-F)
0.6566g, D- fucose (D-F) 0.6566g, sucrose 1.3692g are configured to the sugar juice of 80mM in 50mL volumetric flasks addition PBS
(when 4 DEG C of cold compartment of refrigerator 12 of placement are small).
2) selective enumeration method of fructose：
500 μ L water-solubility fluorescent carbon quantum dots (0.602mg/mL), the APBA of 500 μ L are once added into centrifuge tube
The different types of sugar juice and PBS buffer cumulative volume of (0.03mg/mL), step 1) configuration are 3mL, are made final sugared dense
Spend for 40mM.
To with cuvette in maximum excitation wavelength be that fluoroscopic examination is carried out at 320nm after above-mentioned mixed liquor shaken well.Knot
Fruit sees that Fig. 5, Fig. 5 are the selective enumeration method figure of the fructose of embodiment 2.As shown in Figure 5, the glucose under same concentration, sweet dew
In this ten kinds of sugar of sugar, arabinose, xylose, rhamnose, galactolipin, L-fucose, D- fucoses, fructose, sucrose, fructose makes glimmering
Luminous intensity reduces maximum, and the detection to fructose has selectivity well.
Embodiment 3
To the influence of fructose detection in the presence of glucose：
0.02mM is prepared, the PBS buffer solutions of pH=7.4, take 3mg APBA to be dissolved in 100mLPBS；
500 μ L water-solubility fluorescent carbon quantum dots (0.602mg/mL), the APBA of 500 μ L are once added into centrifuge tube
(0.03mg/mL), fructose soln and PBS buffer cumulative volume are 3mL, make final fructose concentration for 3.33mM conducts pair
According to.
Other conditions are identical consistent with control group, and the glucose solution of three concentration is separately added into fructose soln and makes body
Final fructose concentration is 3.33mM in system, and the concentration of glucose is respectively 1.67mM, 3.33mM, 8.33mM.
To with cuvette in maximum excitation wavelength be that fluoroscopic examination is carried out at 320nm after above-mentioned mixed liquor shaken well.
The result is shown in Fig. 6, Fig. 6 is the influence figure that glucose detects fructose.It is it will be appreciated from fig. 6 that molten in fructose containing same concentrations
In liquid, the glucose of high, normal, basic three concentration is separately added into, the presence of the glucose in mixed system quantitatively detects fructose several
Do not influence.
Embodiment 4
The making of standard curve：
0.02mM is prepared, the PBS buffer solutions of pH=7.4, take 3mg APBA to be dissolved in 100mLPBS；
The accurate 0.4504g fructose standard items that weigh add PBS to be configured to 50mM fructose solns as mother liquor in 50ml volumetric flasks,
It is stand-by when placement cold compartment of refrigerator 12 is small.
500 μ L water-solubility fluorescent carbon quantum dots (0.602mg/mL), the APBA of 500 μ L are once added into centrifuge tube
(0.03mg/mL), the fructose soln of each concentration and PBS buffer cumulative volume are 3mL, make the final fructose concentration be respectively
33.33mM、16.67mM、8.33mM、5mM、3.33mM、2.5mM、1.67mM、1.33mM、0.67mM、0.5mM、0.1mM、
0.05mM、0.083mM.Fluoroscopic examination will be carried out after above-mentioned mixed liquor shaken well at maximum excitation wavelength 320nm, the result is shown in
Fig. 7.For Fig. 7 to be detected figure to different fructose concentrations, it is linear in the range of 0.10-3.33mM to survey fructose concentration,
Minimum detectability is 0.05mM.
Embodiment 5
Actual sample detection is carried out to the fructose in honey:
Take 1mL honey stoste PBS (0.02MpH=7.4) dilutions stand-by；
500 μ L water-solubility fluorescent carbon quantum dots (0.602mg/mL), the APBA of 500 μ L are sequentially added in test tube
(0.03mg/mL), 15 μ L honey (0.07975mg/mL) and then the fructose for adding three concentration gradients respectively.Mixed liquor cumulative volume
For 3mL, wherein the fructose ultimate density added is 0.48mM, 0.6mM, 0.72mM.It will be carried out after above-mentioned mixed liquor shaken well
Detection.As shown in table 1, the sample recovery rate using this method measure fructose is good, and deviation is small.Show in this method detection honey
Fructose accuracy is high.
1 methodology result of table
| Fructose in Honey detectable concentration | Fructose adds concentration | Measured value | The rate of recovery (%) | SD | RSD |
| 0.6mM | 0.48mM | 1.092mM | 102.541% | 0.09210 | 0.090 |
| 0.6mM | 0.6mM | 1.197mM | 99.628% | 0.03906 | 0.140 |
| 0.6mM | 0.72mM | 1.445mM | 117.516% | 0.19309 | 0.164 |
By the standard curve of embodiment 4, the content for measuring Fructose in Honey is 27.11%.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of water-solubility fluorescent carbon quantum dot, it is characterised in that comprise the following steps：
Inkfish juice is prepared into after powder and is mixed with water, carries out hydro-thermal reaction in confined conditions, obtains water soluble fluorescence carbon amounts
Sub- point.
2. preparation method according to claim 1, it is characterised in that the method that the inkfish juice is prepared into powder is：
A) fresh ink anchovy sauce is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge, obtain sediment；
B) obtained sediment is mixed with water, under conditions of 20~30 DEG C stand 8~12 it is small when after centrifuge；
C) repeat step B), the obtained sediment cleaned up is dried and ground, obtains powder.
3. preparation method according to claim 1, it is characterised in that the mass volume ratio of the powder and water is 1g：(15
~20) mL.
4. preparation method according to claim 1, it is characterised in that the temperature of the hydro-thermal reaction is 120~180 DEG C,
When the time of the hydro-thermal reaction is 1~24 small.
5. preparation method according to claim 1, it is characterised in that after the hydro-thermal reaction, further including will be described
After the centrifugation of hydro-thermal reaction product, supernatant liquor is freeze-dried, obtains water-solubility fluorescent carbon quantum dot.
6. a kind of water-solubility fluorescent carbon quantum dot that preparation method is prepared as claimed in any one of claims 1 to 5, wherein, its
It is characterized in that, the water-solubility fluorescent carbon quantum dot has blue-fluorescence under 365nm ultra violet lamps, and in 320nm and 390nm
Maximum emission peak is produced at excitation wavelength respectively.
A kind of 7. method for detecting fructose, it is characterised in that comprise the following steps：
Using fluorescence spectrum, at 320nm, under the conditions of 3- amino phenyl boric acid is existing, the water solubility described in claim 6 is utilized
Fructose in fluorescent carbon quantum dot detection sample to be tested.
8. the method according to the description of claim 7 is characterized in that the sample to be tested is selected from honey.
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| CN108946708A (en) * | 2018-07-02 | 2018-12-07 | 上海理工大学 | A kind of preparation method of high sensitivity graphene quantum dot ultraviolet detector |
| CN110229663A (en) * | 2019-06-26 | 2019-09-13 | 西北大学 | A kind of boration carbon quantum dot and its preparation method and application |
| KR20200112417A (en) * | 2019-03-22 | 2020-10-05 | 가천대학교 산학협력단 | Carbon quantum dots from corn and method for detecting γ-Aminobutyric Acid using the same |
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| CN108946708A (en) * | 2018-07-02 | 2018-12-07 | 上海理工大学 | A kind of preparation method of high sensitivity graphene quantum dot ultraviolet detector |
| CN108929563A (en) * | 2018-09-11 | 2018-12-04 | 广东工业大学 | Water-solubility fluorescent carbon quantum dot is as the application of colorant stabilizer, colorant stabilizer and the method for improving dragon fruit haematochrome stability |
| KR20200112417A (en) * | 2019-03-22 | 2020-10-05 | 가천대학교 산학협력단 | Carbon quantum dots from corn and method for detecting γ-Aminobutyric Acid using the same |
| KR102205066B1 (en) | 2019-03-22 | 2021-01-19 | 가천대학교 산학협력단 | Carbon quantum dots from corn and method for detecting γ-Aminobutyric Acid using the same |
| CN110229663A (en) * | 2019-06-26 | 2019-09-13 | 西北大学 | A kind of boration carbon quantum dot and its preparation method and application |
| CN110229663B (en) * | 2019-06-26 | 2020-08-11 | 西北大学 | Borated carbon quantum dot and preparation method and application thereof |
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