CN109507271A - It is a kind of for the GO/NiCO LDHs catalysis material of glucose detection and the preparation method of electrochemical sensor - Google Patents
It is a kind of for the GO/NiCO LDHs catalysis material of glucose detection and the preparation method of electrochemical sensor Download PDFInfo
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- CN109507271A CN109507271A CN201811381374.7A CN201811381374A CN109507271A CN 109507271 A CN109507271 A CN 109507271A CN 201811381374 A CN201811381374 A CN 201811381374A CN 109507271 A CN109507271 A CN 109507271A
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- G—PHYSICS
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- 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
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- 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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The present invention discloses a kind of for the GO/NiCO LDHs catalysis material of glucose detection and the preparation method of electrochemical sensor.The present invention, which first disperses graphene oxide (GO) in anhydrous methanol, obtains graphene oxide dispersion, GO@ZIF-67 is synthesized using cabaltous nitrate hexahydrate and methylimidazole, then by GO@ZIF-67 and Nickelous nitrate hexahydrate hydrothermal synthesis GO/NiCOLDHs catalysis material, finally the catalysis material solution is dripped to and is handled in clean bare glassy carbon electrode, the electrochemical sensor of GO/NiCO LDHs modification is obtained.The porous structure and regular morphology of the excellent chemical property of present invention combination graphene oxide and MOFs material, it is to sacrifice template with ZIF-67, oriented growth NiCO LDHs catalysis material, for enhancing the stability of electrochemical glucose sensor, widening detection range, reduce testing cost and improve the sensitivity of detection.No enzyme electrochemical sensor is set to show the breakthrough of the raisings such as high stability, high sensitivity, high catalytic property analysis performance.
Description
Technical field
The present invention relates to electrochemical sensor technology field more particularly to enzyme-free glucose detection fields, and in particular to one
Kind is successfully applied to for the GO/NiCO LDHs catalysis material of glucose detection and the preparation method of electrochemical sensor
Blood sugar concentration detects in human body, belongs to functional material and electrochemical sensor technology field.
Background technique
Glucose is substance most commonly seen in daily life, is permitted in the clinical detection of diabetic and food industry etc.
Multi-field quickly and accurately to analyze and detect its content, this has extremely important meaning.Unquestionably, a reason
The necessary matter of utmost importance for developing into sensor industry of the glucose sensor thought, the detection method of glucose has very at present
It is more.For example high performance liquid chromatography, spectrophotometry, Optical Rotation, gas chromatography and electrochemical sensor etc. are relatively more normal
The method seen.Although there are many method of glucose detection, they all cut both ways.Since the structure of glucose is more multiple
It is miscellaneous, the study found that electrochemical sensor has many advantages, such as that detection range is wide and high sensitivity, so electrochemical sensor method is in quotient
Application in industry has broad prospects.
However, electrochemical sensor is also faced with many problems such as in actual detection: stability is relatively poor,
Anti-interference ability is not strong, detection range is relatively narrow etc., this just needs the bimetallics with excellent activity some to electrode face finish
The substances such as hydroxide and graphene construct electrochemical sensor, to increase the current responsing signal of electrode, widen detection
Range, the sensitivity for improving detection.
Graphene is a kind of honeycomb two-dimensional material formed by carbon atom in the form that carbon carbon is conjugated, since its is excellent
Comprehensive performance makes a kind of ideal electrode material, not only has big specific surface area and good electric conductivity, also has
There is the features such as potential window width, electronics transfer impedance is low.Similar with graphene, graphene oxide (GO) is then graphene surface and side
Edge is modified with the Graphene derivative of the oxygen-containing functional groups such as hydroxyl, epoxy group, carbonyl and carboxyl, is the graphite oxide of layer structure
The flaky material obtained by solvation removing or hot lift-off technology.Material is given full play in order to improve the performance of sensor
Performance often organically combines the materials such as some metal nanoparticles, nano-metal-oxide, conducting polymer and graphene, shape
At composite material be applied in electrochemical sensor field, electron transfer rate can be accelerated, significantly improve sensor
The response time is accelerated in selectivity and sensitivity, widens linear detection range and reduces detection limit.
Zeolite imidazole metalloid organic backbone (ZIFs) series material because its with yield height, reconfigurable, pore size,
The series of advantages such as structure and function multiplicity.It is widely used it in electrochemical sensor, the present invention will be in graphene oxide
MOFs material (ZIF-67) is synthesized in substrate, with the porous structure of ZIF-67 material and the pattern of rule, increases electrochemistry
The active site of sensor, enables NiCO LDHs oriented growth on MOF material, improves the electrocatalysis characteristic of sensor,
It is set to play a significant role in terms of glucose detection.
In recent years, glucose sensor is always the hot spot that scholars study, glucose sensor be divided into enzyme sensor with
And without enzyme electrochemical sensor, wherein the stability and importance of enzyme sensor are all poor, and it is easy to be mainly due to enzyme itself
It is affected by environment and expensive, immobilization process is complicated, these disadvantages constrain the application of enzyme sensor to a certain extent
Range keeps the research of no enzyme electrochemical sensor most important, and the key for influencing its performance is opening for electrode modified material
Hair and application, the appearance of nano material will bring immeasurable effect for the progress of sensor.Studies have shown that metal nano material
The advantages that material is learnt well because of its strong adsorption, electrification, large specific surface area, high catalytic efficiency, in the decorative material of electrochemical sensor
Aspect has significant catalytic applications potentiality.The present invention passes through synthesis NiCo duplex metal hydroxide nanometer material (NiCO
LDHs), by the way that nano material and sensor are combined, make no enzyme electrochemical sensor show high stability, high sensitivity,
The breakthrough of the raisings such as high catalytic property analysis performance.
The present invention is directed to the ZIF-67 to grow on graphene oxide to sacrifice template, synthesize bimetallic hydrogen on the template
Oxide (NiCO LDHs), in conjunction with the excellent chemical property of graphene oxide and the porous structure and rule of MOFs material
Pattern, oriented growth NiCO LDHs catalysis material, for enhancing the stability of electrochemical glucose sensor, widening detection model
Enclose, reduce testing cost and improve the sensitivity of detection.Make its in human body blood glucose glucose detection application aspect play
Important role provides more advantageous, significant contribution for effective detection of human diabetes.
Summary of the invention
The purpose of the present invention is to provide a kind of GO/NiCO LDHs catalysis materials and electrification for glucose detection
The preparation method for learning sensor prepares detection sensitivity height using this method, and detection range is big, the low no enzyme electrification of detection limit
Learn sensor.
The present invention, which first disperses graphene oxide (GO) in anhydrous methanol, obtains graphene oxide dispersion, secondly benefit
GO@ZIF-67 is synthesized with cabaltous nitrate hexahydrate and methylimidazole, GO@ZIF-67 and Nickelous nitrate hexahydrate are then subjected to hydro-thermal
GO/NiCO LDHs catalysis material is synthesized, finally the catalysis material ethanol solution is dripped to and is handled in clean bare glassy carbon electrode,
Obtain the electrochemical sensor of GO/NiCO LDHs modification.
The method have the characteristics that the ZIF-67 to grow on graphene oxide is synthesized double on the template to sacrifice template
Metal hydroxides (NiCO LDHs), in conjunction with the excellent chemical property of graphene oxide and the porous structure of MOFs material
And regular morphology, oriented growth NiCO LDHs catalysis material, using the big specific surface area of graphene oxide, good electric conductivity,
Potential window width, electronics transfer impedance is low learns well with metal nano material strong adsorption, electrification, large specific surface area, high catalytic efficiency
The advantages that, so that no enzyme electrochemical sensor is shown the prominent of the raisings such as high stability, high sensitivity, high catalytic property analysis performance
It is broken.
Specific embodiment
Embodiment 1:
(1) 8-20mg graphene oxide (GO) is taken to be scattered in 50ml anhydrous methanol first, 0.5~2h of ultrasound is aoxidized
Graphene dispersing solution A.
(2) 0.498g cabaltous nitrate hexahydrate is taken to be added in dispersion liquid A, 0.5~2h of ultrasound obtains solution B；By 0.656g bis-
Methylimidazole is dissolved in 50ml anhydrous methanol, it is gradually slowly added in solution B, quiet in room temperature after stirring 10~15min
24~48h is set, solution C is obtained, by the solution C collected by suction, and with anhydrous methanol centrifuge washing n times, obtains atropurpureus precipitating
Object, in 60 DEG C be dried in vacuo 12~for 24 hours, obtain product GO@ZIF-67.
(3) 5~20mgGO@ZIF-67 is taken to be scattered in 15ml dehydrated alcohol, 20~30min of ultrasound obtains solution D；By matter
Amount takes appropriate Nickelous nitrate hexahydrate to be dissolved in the dehydrated alcohol of 15ml than 1: 1 (GO@ZIF-67: Nickelous nitrate hexahydrate), is added into
In solution D, 5~10min of ultrasound obtains mixed liquor.Mixed liquor is poured into 50ml autoclave, 80 DEG C of hydro-thermal 6h.It is down to room
Temperature obtains black precipitate by mixed liquor collected by suction, and with dehydrated alcohol centrifuge washing n times, it is dried in vacuo 12 in 60 DEG C~
24h.Obtain GO/NiCO LDHs catalysis material.
(4) glass is modified by the GO/NiCO LDHs catalysis material that GO@ZIF-67 and Nickelous nitrate hexahydrate mass ratio 1: 1 synthesize
Carbon electrode, using the glass-carbon electrode of modification as working electrode, Pt is, to electrode, GCE are reference electrode, selects the hydrogen-oxygen of 1mol/L
Change sodium solution is electrolyte, is assembled into three-electrode electro Chemical system and is tested；When cyclic voltammetry, electrochemical window is selected as
0.1~0.6V, sweeping speed is 50mV/s, and measuring it has apparent oxidation peak in 0.408V when concentration of glucose is 1mmol/L,
0.327V has apparent reduction peak.The range of linearity that detection obtains glucose is 1.0 × 10-7~4.0 × 10-3Mol/L is sensitive
Degree is up to 324 μ A mmol-1cm-2, detection limit (3S/k) is 1.5 × 10-7mol/L。
Embodiment 2:
The mass ratio for changing GO@ZIF-67 and Nickelous nitrate hexahydrate is 1: 2, and measuring it in concentration of glucose is 1mmol/L
When in 0.438V have apparent oxidation peak, have apparent reduction peak in 0.348V.
Embodiment 3:
The mass ratio for changing GO@ZIF-67 and Nickelous nitrate hexahydrate is 1: 3, and measuring it in concentration of glucose is 1mmol/L
When in 0.481V have apparent oxidation peak, have apparent reduction peak in 0.362V.
Claims (10)
1. it is a kind of for the GO/NiCO LDHs catalysis material of glucose detection and the preparation method of electrochemical sensor, it is special
Sign be the electrochemical sensor preparation method through the following steps that building:
It first disperses graphene oxide (GO) in anhydrous methanol and obtains graphene oxide dispersion, followed by utilize six hydrations
Cobalt nitrate and methylimidazole synthesize GO@ZIF-67, and GO@ZIF-67 and Nickelous nitrate hexahydrate are then carried out hydrothermal synthesis GO/
The catalysis material solution is finally dripped to and is handled in clean bare glassy carbon electrode, obtains GO/NiCO by NiCO LDHs catalysis material
The electrochemical sensor of LDHs modification.
2. electrochemical sensor as described in claim 1, it is characterised in that: 8~20mg graphene oxide (GO) is taken to be scattered in
50ml anhydrous methanol, 0.5~2h of ultrasound, obtains graphene oxide dispersion.
3. electrochemical sensor as described in claim 1, it is characterised in that: by cabaltous nitrate hexahydrate and methylimidazole quality
Than being separately added into graphene oxide solution for 1: 1~1: 3；Ultrasonic agitation stands certain time, collected by suction, centrifuge washing n
It is secondary, obtain atropurpureus sediment, in 60 DEG C be dried in vacuo 12~for 24 hours, obtain product GO@ZIF-67.
4. electrochemical sensor as claimed in claim 3, it is characterised in that: 0.5~2h of ultrasound is stored at room temperature 24~48h.
5. electrochemical sensor as claimed in claim 3, it is characterised in that: eluant, eluent can be anhydrous methanol, deionized water,
Dehydrated alcohol.
6. electrochemical sensor as described in claim 1, it is characterised in that: GO@ZIF-67 and Nickelous nitrate hexahydrate mass ratio
15ml dehydrated alcohol is scattered in respectively for 1: 1~1: 5, after 5~10min of ultrasound, in 50ml autoclave hydro-thermal reaction.It is down to
Room temperature, collected by suction, centrifuge washing n times obtain black precipitate, in 60 DEG C be dried in vacuo 12~for 24 hours.Obtain GO/NiCO
LDHs catalysis material.
7. electrochemical sensor as claimed in claim 6, it is characterised in that: hydro-thermal reaction reacts 1~8h at 60~90 DEG C.
8. electrochemical sensor as claimed in claim 6, it is characterised in that: eluant, eluent can be anhydrous methanol, deionized water,
Dehydrated alcohol.
9. electrochemical sensor as described in claim 1, it is characterised in that: use glass-carbon electrode (GCE, 3mm) on chamois leather
A- aluminum oxide polishing powder (d50: 50nm) polishes 2~5min, is then cleaned by ultrasonic 5~10min with secondary distilled water, uses N2It blows
It is dry, obtain bare glassy carbon electrode.
10. the electrochemical sensor as described in claim 1~6, it is characterised in that: urged with the GO/NiCO LDHs of 5~10uL
Change in material ethanol solution modification bare glassy carbon electrode, 1~3uL naphthols is added dropwise, the electrochemistry for obtaining GO/NiCO LDHs modification passes
Sensor.
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|---|---|---|---|---|
| CN111122533A (en) * | 2020-04-01 | 2020-05-08 | 烟台职业学院 | ZIF nano enzyme and preparation method and application thereof |
| CN111239214A (en) * | 2020-03-25 | 2020-06-05 | 吉林大学 | Three-electrode type Pb (II) and Cu (II) electrochemical sensor, preparation method and application thereof |
| CN112067678A (en) * | 2020-09-22 | 2020-12-11 | 哈尔滨理工大学 | Electrochemical sensing electrode of selenium functionalized honeycomb porous carbon nanosheet |
| CN112505118A (en) * | 2020-11-18 | 2021-03-16 | 山西大学 | Electrochemical sensor for detecting glucose and preparation method thereof |
| CN113332956A (en) * | 2021-04-25 | 2021-09-03 | 佛山水业集团高明供水有限公司 | Micro solid phase extraction adsorbent for detecting smelly substances in water and preparation method thereof |
| CN113707466A (en) * | 2021-08-30 | 2021-11-26 | 新余学院 | Graphene oxide/ammonium nickel phosphate composite electrode material and preparation method and application thereof |
| CN114235920A (en) * | 2021-12-20 | 2022-03-25 | 天津工业大学 | NiCo LDH/NiCoS @ C composite material and preparation method and application thereof |
| CN114324516A (en) * | 2021-11-29 | 2022-04-12 | 郑州轻工业大学 | Preparation method of nano composite electrode material for detecting nitro compound with high sensitivity |
| CN114965627A (en) * | 2022-05-26 | 2022-08-30 | 新余学院 | Reduced graphene oxide/ammonium nickel phosphate/GCE composite electrode and preparation method and application thereof |
| CN115165990A (en) * | 2022-06-27 | 2022-10-11 | 江南大学 | Electrochemical sensing analysis method for detecting bisphenol A |
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Cited By (15)
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| CN111239214A (en) * | 2020-03-25 | 2020-06-05 | 吉林大学 | Three-electrode type Pb (II) and Cu (II) electrochemical sensor, preparation method and application thereof |
| CN111239214B (en) * | 2020-03-25 | 2021-05-25 | 吉林大学 | Three-electrode type Pb (II) and Cu (II) electrochemical sensor, preparation method and application thereof |
| CN111122533A (en) * | 2020-04-01 | 2020-05-08 | 烟台职业学院 | ZIF nano enzyme and preparation method and application thereof |
| CN112067678A (en) * | 2020-09-22 | 2020-12-11 | 哈尔滨理工大学 | Electrochemical sensing electrode of selenium functionalized honeycomb porous carbon nanosheet |
| CN112505118B (en) * | 2020-11-18 | 2022-03-18 | 山西大学 | Electrochemical sensor for detecting glucose and preparation method thereof |
| CN112505118A (en) * | 2020-11-18 | 2021-03-16 | 山西大学 | Electrochemical sensor for detecting glucose and preparation method thereof |
| CN113332956A (en) * | 2021-04-25 | 2021-09-03 | 佛山水业集团高明供水有限公司 | Micro solid phase extraction adsorbent for detecting smelly substances in water and preparation method thereof |
| CN113707466A (en) * | 2021-08-30 | 2021-11-26 | 新余学院 | Graphene oxide/ammonium nickel phosphate composite electrode material and preparation method and application thereof |
| CN114324516A (en) * | 2021-11-29 | 2022-04-12 | 郑州轻工业大学 | Preparation method of nano composite electrode material for detecting nitro compound with high sensitivity |
| CN114324516B (en) * | 2021-11-29 | 2023-09-15 | 郑州轻工业大学 | Preparation method of nanocomposite electrode material for detecting nitro compound with high sensitivity |
| CN114235920A (en) * | 2021-12-20 | 2022-03-25 | 天津工业大学 | NiCo LDH/NiCoS @ C composite material and preparation method and application thereof |
| CN114965627A (en) * | 2022-05-26 | 2022-08-30 | 新余学院 | Reduced graphene oxide/ammonium nickel phosphate/GCE composite electrode and preparation method and application thereof |
| CN114965627B (en) * | 2022-05-26 | 2024-02-02 | 新余学院 | Reduced graphene oxide/nickel ammonium phosphate/GCE composite electrode and preparation method and application thereof |
| CN115165990A (en) * | 2022-06-27 | 2022-10-11 | 江南大学 | Electrochemical sensing analysis method for detecting bisphenol A |
| CN115165990B (en) * | 2022-06-27 | 2023-08-08 | 江南大学 | Electrochemical sensing analysis method for detecting bisphenol A |
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