CN107102052A - Based on the uric acid electrochemical sensor containing active copper carbon point and its application - Google Patents
Based on the uric acid electrochemical sensor containing active copper carbon point and its application Download PDFInfo
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- CN107102052A CN107102052A CN201710279857.5A CN201710279857A CN107102052A CN 107102052 A CN107102052 A CN 107102052A CN 201710279857 A CN201710279857 A CN 201710279857A CN 107102052 A CN107102052 A CN 107102052A
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- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229940116269 uric acid Drugs 0.000 title claims abstract description 41
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 title claims abstract description 40
- AHADSRNLHOHMQK-UHFFFAOYSA-N methylidenecopper Chemical compound [Cu].[C] AHADSRNLHOHMQK-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 239000010949 copper Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000004070 electrodeposition Methods 0.000 claims abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229920000193 polymethacrylate Polymers 0.000 claims description 5
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 4
- 241001481789 Rupicapra Species 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 4
- 125000004122 cyclic group Chemical group 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 239000010985 leather Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052802 copper Inorganic materials 0.000 abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000027756 respiratory electron transport chain Effects 0.000 abstract description 2
- 238000000502 dialysis Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 238000002484 cyclic voltammetry Methods 0.000 description 6
- 239000008055 phosphate buffer solution Substances 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 229960003638 dopamine Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000011896 sensitive detection Methods 0.000 description 2
- 238000004832 voltammetry Methods 0.000 description 2
- 208000010444 Acidosis Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000000627 alternating current impedance spectroscopy Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000003759 clinical diagnosis Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 230000002969 morbid Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- -1 potassium ferricyanide Chemical compound 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 150000007968 uric acids Chemical class 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The present invention is disclosed based on the uric acid electrochemical sensor containing active copper carbon point and its application.The present invention will be enriched in the high molecular polymer of carboxyl, is added to containing cupric salt in reaction vessel, be placed in hydrothermal reaction kettle, and 2~18h is reacted at 200~240 DEG C, and centrifugation, dialysis purification is obtained containing active copper carbon dots solution；Using three-electrode system, using glass-carbon electrode as working electrode, platinum electrode is to electrode, saturated calomel electrode is reference electrode, above-mentioned pretreated glass-carbon electrode is inserted in the above-mentioned solution containing active copper carbon point, 50~500mV/s of potential range using electrodeposition process in 0~2V sweeps scan round under speed.Compared with prior art, the present invention not only has the big specific surface area of carbon point and high electron transport rate using containing this nano material of active copper carbon point, and also active copper is to the facilitation of the electron transfer rate of matrix on electrode interface and the very strong selectivity to uric acid.
Description
Technical field
The invention belongs to electrochemica biological sensor technical field, and in particular to based on the carbon point electrochemistry containing active copper
Sensor and its application, realize the selective Sensitive Detection to uric acid.
Background technology
Uric acid is the metabolite of human body purine, can cause urarthritis, high urine if too high levels in human body
The disease such as acidaemia and Lesh Nyan syndromes.Recently as the raising of people's quality of life, our people takes the photograph from food
The purine content taken is improved, and increasing people is in the too high sub-health state of uric acid even morbid state.Therefore, in human body
The accurate detection of uric acid concentration is particularly important in clinical diagnosis field.
The assay method of current uric acid concentration mainly has chromatography, AAS, fluorescence method, chemoluminescence method, electrification
Method.Wherein electrochemical method has the advantages that the good, sensitivity of selectivity is high, simple to operate and with low cost and is widely used in
The measure of uric acid.But the method for prior art electrochemical sensor detection uric acid mainly runs into two problems：On the one hand, it is traditional
The current potential of its oxidizing potential and ascorbic acid is approached on electrode, is easily disturbed by ascorbic acid；On the other hand, uric acid is detected
Sensitivity limited can not meet demand.
The content of the invention
It is an object of the present invention to solve the technical problem in the presence of prior art to be based on containing living there is provided one kind
Property copper carbon point (Cu-CDs) uric acid electrochemica biological sensor, by the selectivity of active copper and carbon point improving above sensitivity
Contribution combine.Finally realize the highly sensitive detection of selectivity to uric acid, with selectivity good, high sensitivity stability and
Preparation technology is simple, low cost and other advantages.
The present invention provide based on the carbon point electrochemical sensor containing active copper, prepared using following methods step and
Into：
1) active copper carbon point is contained using hydro-thermal method one-step synthesis：
Will be enriched in the high molecular polymer of carboxyl, be added to containing cupric salt in reaction vessel, then add 50ml go from
Sub- water dilution, mixed reaction solution is obtained after being well mixed；Mixed reaction solution is poured into hydrothermal reaction kettle again, at 200~240 DEG C
2~18h is reacted, mixed liquor is obtained；Gained mixed liquor 13000rpm is centrifuged to the bulky grain residue removed in solution for 30 minutes；With
Molecular weight dialyses 10~30h to reach the purpose of purifying for 500~3000D bag filter, is finally kept in dark place, obtains at 4 DEG C
To the solution containing active copper carbon point；
Described is Cu (NO containing cupric salt3)2、CuCl2、CuSO4Deng；
Described high molecular polymer is sodium polymethacrylate (PMAA), Sodium Polyacrylate (PAAS) etc.；
Described high molecular polymer is 1 with the mass ratio containing cupric salt：0.02~0.1；
The concentration of bivalent cupric ion is 1~10.2mgmL in described mixed reaction solution-1。
2) preparation of electrochemica biological sensor：
1. the pretreatment of glass-carbon electrode：Be respectively 1.0 with particle diameter, 0.3,0.05 μm of alumina powder coordinate chamois leather to polish
Electrode, in 0.65mM (concentration range is in 0.1mmol~1mmol) K3[Fe(CN)6]/K4[Fe(CN)6] carry out in solution
Cyclic voltammetric is characterized, after the peak difference △ Ep ＜ 75mV of oxidation peak and reduction peak, then uses acetone, ethanol and deionized water successively
It is cleaned by ultrasonic, is finally dried up with nitrogen stand-by.
2. the preparation of electrochemica biological sensor：Using three-electrode system, using glass-carbon electrode as working electrode, platinum electrode
For to electrode, saturated calomel electrode is reference electrode, above-mentioned pretreated glass-carbon electrode is inserted into containing for step (1) preparation
In the solution of active copper carbon point, 50~500mV/s of potential range using electrodeposition process in 0~2V sweeps scan round 2 under speed
~20 circles, so as to be made based on the electrochemica biological sensor containing active copper carbon point.
It is a further object to provide above-mentioned based on the electrochemica biological sensor containing active copper carbon point, in inspection
The application surveyed on uric acid, specifically includes following steps：
1) using phosphate buffer solution as bottom liquid, different pH uric acid prepare liquid is configured, by electrochemica biological sensor
Three electrodes connection electrochemical workstation is inserted in the solution, is tested, is obtained with electrochemical response using cyclic voltammetry
Cyclic voltammetry curve, contrast uric acid peak current size and pH relation, find out optimal pH.
2) using phosphate buffer solution as bottom liquid, uric acid prepare liquid is configured, three electrodes of electrochemica biological sensor are connected
Connect electrochemical workstation to insert in the solution, change sweep speed and tested using cyclic voltammetry, obtained with electrochemistry
The relation of the cyclic voltammetry curve of response, contrast uric acid peak current size and sweep speed, finds out and most preferably sweeps fast value.
3) using phosphate buffer solution as bottom liquid, a series of different uric acid prepare liquids under optimal pHs are configured, by electrochemistry
In the three electrodes connection electrochemical workstation insertion prepare liquid of biology sensor, voltammetry is used under optimum scanning speed
Tested, obtain the voltage-to-current working curve with electrochemical response characteristic peak, therefrom obtain concentration-peak current relation
Working curve.
Compared with prior art, the present invention, which is utilized, not only has the big ratio of carbon point containing this nano material of active copper carbon point
Surface area and high electron transport rate, facilitation of the also active copper to the electron transfer rate of matrix on electrode interface
And to the very strong selectivity of uric acid.Biology sensor is prepared based on this principle, realized to uric acid sensitivity, specificity
With the measure of stability.
Brief description of the drawings
Fig. 1 is the experimental principle schematic diagram that uric acid is detected based on Cu-CDs electrochemical sensors；
(illustration is Cu-CDs under ultra violet lamp to the fluorescence spectrum and ultraviolet-visible absorption spectroscopy that Fig. 2 is Cu-CDs
Picture)；
Fig. 3 is the ac impedance spectroscopy of different modifying electrode；
Fig. 4 is cyclic voltammogram of the Different electrodes in uric acid solution；
Fig. 5 is influence figures of the pH to this experiment；
Fig. 6 is influence figure of the sweep speed to this experiment；
Fig. 7 is influence figure of the uric acid of various concentrations to this experiment；
Fig. 8 is the uric acid of various concentrations and the linear relationship chart of peak current；
Fig. 9 be this method to dopamine, the selective comparison diagram of ascorbic acid and uric acid.
Embodiment
The present invention is further analyzed with reference to specific embodiments and the drawings.
Embodiment 1
Based on the preparation method of the carbon point electrochemica biological sensor containing active copper, comprise the following steps：
A, the preparation containing active copper carbon point：Contain the carbon point of active copper using hydro-thermal method one-step synthesis：Weigh first
2.5g PMAA and 50mg Cu (NO3)2In beaker, the dilution of 50ml deionized waters, uniform thermal response of falling back to be mixed are added
In kettle, 240 DEG C of reaction 9h.Products therefrom 13000rpm is centrifuged to the bulky grain residue removed in solution for 30 minutes.Use molecular weight
12h is dialysed to reach the purpose of purifying for 1000D bag filter, is finally kept in dark place at 4 DEG C.Using fluorescence spectrum and ultraviolet
Visible absorption spectra is characterized to what is obtained containing active copper carbon point, as a result as shown in Figure 2.
B, glass-carbon electrode pretreatment：Be respectively 1.0 with particle diameter, 0.3,0.05 μm of alumina powder coordinate chamois leather to polish
Electrode, in 0.65mM K3[Fe(CN)6]/K4[Fe(CN)6] cyclic voltammetric sign is carried out in solution, when oxidation peak and reduction peak
After peak difference △ Ep ＜ 75mV, then finally dried up successively with acetone, ethanol and deionized water ultrasonic cleaning with nitrogen stand-by.
C, electrochemica biological sensor preparation：Using three-electrode system, using glass-carbon electrode as working electrode, platinum electrode
For to electrode, saturated calomel electrode is reference electrode, by above-mentioned pretreated glass-carbon electrode insert prepared by step 1 containing living
In the carbon dots solution of property copper, using electrodeposition process 0~2V potential range 100mV/s sweep speed under scan round 10 enclose, from
And be made based on the electrochemica biological sensor containing active copper carbon point.
Under experiment condition same as Example 1, electrochemica biological sensor is placed in potassium ferricyanide solution, 0.01
Scanned in~100KHz range of scanned frequencies, as a result as shown in Figure 3.
Under experiment condition same as Example 1, electrochemica biological sensor is placed in 0.1mol/L PBS solutions (pH
7.0) in, carried out in -0.4~0.6 potential range, sweeping for 100mV/s is carried out under speed, records corresponding cyclic voltammogram,
As a result it is as shown in Figure 4.
Embodiment 2
By 50mg Cu (NO3)2It is changed into 1500mg Cu (NO3)2, other conditions be the same as Example 1, which is made, to be based on containing active copper
The electrochemica biological sensor of carbon point.
Embodiment 3
By 50mg Cu (NO3)2It is changed into 36.4mg CuCl2, other conditions be the same as Example 1, which is made, to be based on containing active copper carbon
The electrochemica biological sensor of point.
Embodiment 4
By 50mg Cu (NO3)2It is changed into 1092mg CuCl2, other conditions be the same as Example 1, which is made, to be based on containing active copper carbon
The electrochemica biological sensor of point.
Embodiment 5
By 50mg Cu (NO3)2It is changed into 42.6mg CuSO4, other conditions be the same as Example 1, which is made, to be based on containing active copper carbon
The electrochemica biological sensor of point.
Embodiment 6
By 50mg Cu (NO3)2It is changed into 1278mg CuSO4, other conditions be the same as Example 1, which is made, to be based on containing active copper carbon
The electrochemica biological sensor of point.
Embodiment 7
The concentration of uric acid is detected using the sensor of above-mentioned preparation, as shown in Figure 1：
A, prepare uric acid solution：The uric acid of purchase is dissolved with phosphate buffer solution, it is 100 μm of ol/L to be configured to concentration
Solution, 4 DEG C of preservations are stand-by；The preparation of 0.1mol/L phosphate buffer solutions (PBS)：Use NaH2PO4, Na2HPO4Match somebody with somebody with KCl
System, and use 0.10mol/L H3PO4Or NaOH adjusts pH value, 4 DEG C of preservations are stand-by.
B, glass-carbon electrode pretreatment：Be respectively 1.0 with particle diameter, 0.3,0.05 μm of alumina powder coordinate chamois leather to polish
Electrode, in 0.65mM K3[Fe(CN)6]/K4[Fe(CN)6] cyclic voltammetric sign is carried out in solution, when oxidation peak and reduction peak
After peak difference △ Ep ＜ 75mV, then finally dried up successively with acetone, ethanol and deionized water ultrasonic cleaning with nitrogen stand-by.
C, electrochemica biological sensor preparation：Using three-electrode system, using glass-carbon electrode as working electrode, platinum electrode
For to electrode, saturated calomel electrode is reference electrode, above-mentioned pretreated glass-carbon electrode is inserted into the step A of embodiment 1 and prepared
The carbon dots solution containing active copper in, the potential range 100mV/s using electrodeposition process in 0~2V sweeps scan round under speed
10 circles, so that the electrochemica biological sensor based on the carbon point containing active copper is made.
D, using phosphate buffer solution (pH=7.0) as bottom liquid, configure a series of uric acid prepare liquid of various concentrations, will be upper
State in electrochemica biological sensor connection electrochemical workstation insertion prepare liquid, letting nitrogen in and deoxidizing, under 100mV/s sweep speed
Use voltammetry tested (parameter for：Sweep speed 50mV/s, amplification 0.05V, pulse width 0.05s, scan model
Enclose -0.12~0.25V).The peak current measured sets up linear relationship (Fig. 7 and Fig. 8) with concentration, is then tested under the same terms,
The peak current of unknown concentration uric acid is measured, the concentration of uric acid is drawn according to the concentration of foundation-peak current relation working curve.
Embodiment 8
Change the pH value of cushioning liquid, other step be the same as Examples 2, influence of the pH value to this experiment is as shown in Figure 5；
Change sweep speed, other step be the same as Examples 2, influence of the sweep speed to this experiment is as shown in Figure 6；
Embodiment 9
Detection object uric acid is changed to ascorbic acid and dopamine respectively, in same experimental example 2 under the same conditions, as a result such as
Shown in Fig. 9.
Above-described embodiment is not the limitation for the present invention, and the present invention is not limited only to above-described embodiment, as long as meeting
Application claims, belong to protection scope of the present invention.
Claims (6)
1. based on the uric acid electrochemical sensor containing active copper carbon point, it is characterised in that be prepared from using following methods：
Step (1), contain active copper carbon point using hydro-thermal method one-step synthesis：
It will be enriched in the high molecular polymer of carboxyl, be added to containing cupric salt in reaction vessel, then add deionized water dilution,
Mixed reaction solution is obtained after well mixed；Mixed reaction solution is poured into hydrothermal reaction kettle again, at 200~240 DEG C react 2~
18h, obtains mixed liquor, and centrifugation removes bulky grain residue；With molecular weight for 500~3000D bag filter dialyse 10~30h with up to
To the purpose of purifying, it is kept in dark place, obtains the solution containing active copper carbon point；
Step (2), the preparation of electrochemica biological sensor：
The pretreatment of 2.1 glass-carbon electrodes：Respectively with alumina powder coordinate chamois leather polishing electrode, concentration be 0.1mmol~
1mmol K3[Fe(CN)6]/K4[Fe(CN)6] cyclic voltammetric sign is carried out in solution, when oxidation peak and the peak difference of reduction peak
After △ Ep ＜ 75mV, then finally dried up successively with acetone, ethanol and deionized water ultrasonic cleaning with nitrogen stand-by；
The preparation of 2.2 electrochemica biological sensors：Using three-electrode system, using glass-carbon electrode as working electrode, platinum electrode is
To electrode, saturated calomel electrode is reference electrode, and above-mentioned pretreated glass-carbon electrode is inserted into containing for step (1) preparation and lived
In the solution of property copper carbon point, using electrodeposition process 0~2V 50~500mV/s of potential range sweep scan round 2 under speed~
20 circles, so as to be made based on the electrochemica biological sensor containing active copper carbon point.
2. as claimed in claim 1 based on the uric acid electrochemical sensor containing active copper carbon point, it is characterised in that step (1)
Described is Cu (NO containing cupric salt3)2、CuCl2Or CuSO4。
3. as claimed in claim 1 based on the uric acid electrochemical sensor containing active copper carbon point, it is characterised in that step (1)
Described rich carboxylic high molecular polymer is sodium polymethacrylate (PMAA) or Sodium Polyacrylate (PAAS).
4. as claimed in claim 1 based on the uric acid electrochemical sensor containing active copper carbon point, it is characterised in that step (1)
Described rich carboxylic high molecular polymer is 1 with the mass ratio containing cupric salt：0.02~0.1.
5. as claimed in claim 1 based on the uric acid electrochemical sensor containing active copper carbon point, it is characterised in that step (1)
The concentration of bivalent cupric ion is 1~10.2mgmL in described mixed reaction solution-1。
6. as claimed in claim 1 based on the uric acid electrochemical sensor containing active copper carbon point, answering on detection uric acid
With.
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| CN109705858A (en) * | 2019-01-04 | 2019-05-03 | 河南大学 | A kind of preparation method and applications of cupric carbon dots |
| CN110339357A (en) * | 2019-02-28 | 2019-10-18 | 安徽大学 | Copper ion doped carbon dots, preparation and its application as photosensitizer for photodynamic therapy |
| CN112458518A (en) * | 2020-11-20 | 2021-03-09 | 昆明理工大学 | Preparation method of high-conductivity copper-based composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705858A (en) * | 2019-01-04 | 2019-05-03 | 河南大学 | A kind of preparation method and applications of cupric carbon dots |
| CN109705858B (en) * | 2019-01-04 | 2020-05-01 | 河南大学 | Preparation method and application of copper-containing carbon dots |
| CN110339357A (en) * | 2019-02-28 | 2019-10-18 | 安徽大学 | Copper ion doped carbon dots, preparation and its application as photosensitizer for photodynamic therapy |
| CN110339357B (en) * | 2019-02-28 | 2021-04-13 | 安徽大学 | Copper ion doped carbon dot, preparation and application thereof as photodynamic therapy photosensitizer |
| CN112458518A (en) * | 2020-11-20 | 2021-03-09 | 昆明理工大学 | Preparation method of high-conductivity copper-based composite material |
| CN112458518B (en) * | 2020-11-20 | 2023-07-28 | 昆明理工大学 | Preparation method of high-conductivity copper-based composite material |
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