CN106610400A - Method for detecting amaranth in food by using porous graphene - Google Patents
Method for detecting amaranth in food by using porous graphene Download PDFInfo
- Publication number
- CN106610400A CN106610400A CN201710003057.0A CN201710003057A CN106610400A CN 106610400 A CN106610400 A CN 106610400A CN 201710003057 A CN201710003057 A CN 201710003057A CN 106610400 A CN106610400 A CN 106610400A
- Authority
- CN
- China
- Prior art keywords
- amaranth
- porous graphene
- gce
- powder
- electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 240000001592 Amaranthus caudatus Species 0.000 title claims abstract description 58
- 235000009328 Amaranthus caudatus Nutrition 0.000 title claims abstract description 57
- 235000012735 amaranth Nutrition 0.000 title claims abstract description 57
- 239000004178 amaranth Substances 0.000 title claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 235000013305 food Nutrition 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 239000000523 sample Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 238000002604 ultrasonography Methods 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000007853 buffer solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000002484 cyclic voltammetry Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000012417 linear regression Methods 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000003950 stripping voltammetry Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 230000002708 enhancing effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- AMDUMQZTBRMNMG-UHFFFAOYSA-N nickel nitric acid Chemical compound [Ni].O[N+]([O-])=O AMDUMQZTBRMNMG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000006467 substitution reaction Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000003139 buffering effect Effects 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 230000005518 electrochemistry Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000012546 transfer Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 235000020095 red wine Nutrition 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 238000000835 electrochemical detection Methods 0.000 description 2
- 238000004365 square wave voltammetry Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 241001481789 Rupicapra Species 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000021185 dessert Nutrition 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000141 square-wave voltammogram Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004832 voltammetry Methods 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
-
- 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 invention relates to a method for detecting amaranth in food by using porous graphene, belonging to the field of analytical chemistry or food safety. According to the invention, porous graphene is prepared by using a metal etching method; dispersion liquid of porous graphene is dispensed on the surface of a glassy carbon electrode so as to prepare a porous graphene modified glassy carbon electrode; and since porous graphene has a large specific surface area, high conductivity, strong adsorption capability and good mass transfer effect, the porous graphene modified glassy carbon electrode is used for detecting amaranth in food in experiments. The detection method provided by the invention has the advantages of high sensitivity, low detection limit, easiness and accurate results.
Description
Technical field
The present invention relates to electro chemical analysis measuring technology or field of food safety, specifically with metal etching method system
Standby porous graphene is electrode modified material, using the method for amaranth in electrochemical means detection food.
Background technology
Using the development of Electrochemical Detection food additive, medicine and biomolecule cause a series of biosensors,
Food senses the quick appearance with environmental sensor.Because its high sensitivity, price are low high, simple to operate and easily small-sized
The advantages of change, electrochemical measuring technique has been successfully applied to protein analyses, biological monitoring, pharmaceutical analysiss and food point
The fields such as analysis.In order to cause the pigments such as everybody appetite, amaranth to be often added in the food such as dessert, confection, beverage.Root
Organize according to food hygiene（FAO）And World Health Organization (WHO)（WHO）Regulation, the daily intaking amount of amaranth is 0 ~ 0.5mg/kg.So
And, in order to cause the desire for consumer goods of consumer to increase sudden huge profits, illegal retailer Jing is often added to excessive amaranth in product.
Therefore, realize extremely urgent to the efficient detection of amaranth in food.Certainly, the performance of electrochemical sensor excellent properties is depended on
In the design of electrode material.Porous graphene is due to big surface area and high electric conductivity, becoming a kind of function admirable
Electrode material.
The content of the invention
Based on above-mentioned prior art, it is an object of the invention to provide a kind of detected using porous graphene modified glassy carbon electrode
The method of amaranth.Porous graphene modified glassy carbon electrode sensor is prepared for using metal etching method, using porous graphite
The big specific surface area and fabulous mass transfer effect of alkene, to the amaranth in food quick detection has been carried out.
The present invention adopts the following technical scheme that realization：
The method of amaranth, comprises the steps in a kind of utilization porous graphene detection food：
（1）, porous graphene prepare
Nitric acid nickel by powder is dissolved in deionized water, then under agitation graphite oxide GO solution is added to into above-mentioned nitre
In sour nickel solution, it is 10 to control GO with the mass ratio of Ni elements：1；After by above-mentioned mixed solution ultrasound, mixed solution is turned rapidly
In shift-in freeze dryer, in less than liquid nitrogen vacuum freezing 48h is used at a temperature of 0 DEG C, then by the powder for obtaining with 10 DEG C/
Min speed is heated to 800 DEG C in tube furnace from room temperature, and keeps 1h in the Ar atmosphere of flowing, has obtained black solid powder
End；Finally, after cleaning being carried out to the black powder for obtaining so that the hole of graphenic surface displays with dilute hydrochloric acid, spend from
Sub- water washing, vacuum drying is obtained porous graphene PG.
（2）, porous graphene modified glassy carbon electrode PG/GCE
By glass-carbon electrode GCE α-Al2O3The turbid liquid of powder makees polishing, then cleans up glass-carbon electrode；PG is dispersed in into height
In pure water and ultrasound, PG dispersion liquids are obtained, PG dispersant liquid drops are coated in the GCE surfaces that clean up and are dried under infrared lamp and obtained
Obtain electrode PG/GCE.
（3）, using porous graphene modified glassy carbon electrode detection food in amaranth
Using PG/GCE as working electrode, used as reference electrode, platinum electrode is used as auxiliary electrode, composition three for saturated calomel electrode
Electrode system；The three-electrode system is initially positioned at containing 5.0 × 10-6mol·L-1The pH of amaranth be 7.0 BR buffering it is molten
In liquid, the stirring enrichment 210s under open-circuit condition after standing 10s, utilizes cyclic voltammetric in the potential range of 0.5V to 1.0V
Method is scanned, and records cyclic voltammetry curve, studies electrochemical behavior of the amaranth on PG/GCE surfaces, it is known that amaranth exists
Oxidation peak current on PG/GCE obtains significantly enhancing；Further with square wave stripping voltammetry 0.5V to 1.0V electricity
The amaranth of variable concentrations is scanned in the range of position, the parameter setting of square wave voltammetry is as follows：Current potential increment is 4mV；Amplitude is
25mV；Frequency is 10Hz；Record square wave volt-ampere curve, and read the oxidation peak current value of amaranth；The data obtained Jing statistics after,
As abscissa, peak point current is vertical coordinate to concentration with amaranth, 5.0 × 10-9mol/L~1.0×10-6In the range of mol/L
Standard curve is drawn, detection is limited to 0.8 × 10-10Mol/L, extrapolate the corresponding equation of linear regression of amaranth for I (A)=
45.77 × C (M) -0.18, the equation is used for determining the concentration of amaranth in actual sample.
（4）, actual sample detection
Take sample to be placed in volumetric flask, with the BR buffer solution constant volumes that pH is 7.0；According to step（3）Identical electrochemistry is surveyed
Method for testing is that square wave stripping voltammetry is tested testing sample solution, to obtain solution to be measured in amaranth oxidation peak electricity
Flow valuve, by resulting current value substitution step（3）Calculated in the equation of linear regression for obtaining, drawn detected sample
The concentration of middle amaranth.
The porous graphene synthesized in the present invention has the hole of nano-scale, and hole is uniform, and this structure causes this
When porous graphene is as electrode material, not only with big specific surface area, while also good mass transfer effect, can be abundant
The peculiar property of two-dimentional porous graphene is played, the electrode material of preparation significantly improves the electrochemical response to amaranth.With
The technology of existing Electrochemical Detection amaranth is compared, and more preferably, test limit is lower, and simple to operate, saves time for the method Detection results,
Have a extensive future.
Description of the drawings
Fig. 1 represents the TEM figures of porous graphene of the present invention.
Fig. 2 represents GCE electrodes (b), G/GCE electrodes (c) and PG/GCE electrodes (d) comprising 5.0 × 10-6mol·L-1Herba Amaranthi tricoloriss
The red 0.1molL of dish-1PH be cyclic voltammogram in 7.0 BR buffer solution；Represent that PG/GCE electrodes (a) is not including
The 0.1molL of amaranth-1PH be cyclic voltammogram in 7.0 BR buffer solution, scanning speed is 100mVs-1。
Fig. 3 a represent square wave voltammogram of the amaranth of variable concentrations in the present invention on PG/GCE electrodes.
Fig. 3 b are represented in the present invention with amaranth concentration as abscissa, linear relationship chart of the peak point current as vertical coordinate.
Specific embodiment
The specific embodiment of the present invention is further illustrated below.
The method of amaranth, comprises the steps in a kind of utilization porous graphene detection food：
（1）, porous graphene prepare
By a certain amount of nickel nitrate（II）Powder is dissolved in 15mL deionized waters, then by 10mL concentration is under agitation
4mg·mL -1Graphite oxide（GO）Solution is added in above-mentioned nickelous nitrate solution.It is 10 that GO is controlled with the mass ratio of Ni elements：
1.After by above-mentioned mixed solution ultrasound 10min, mixed solution is transferred in freeze dryer rapidly, in the temperature less than 0 DEG C
Lower use liquid nitrogen vacuum freezing 48h, is then heated to 800 in tube furnace with 10 DEG C/min speed by the powder for obtaining from room temperature
DEG C, and 1h is kept in the Ar atmosphere of flowing, obtain black solid powder.Finally, with dilute hydrochloric acid to the black powder that obtains
After cleaning is carried out so that the hole of graphenic surface is displayed, a large amount of deionized water wash are used, be vacuum dried, porous stone is obtained
Black alkene（PG）.Accompanying drawing 1 is schemed for the TEM of PG, and the mass ratio of adjustment GO and Ni can be passed through in this preparation method to adjust porous stone
The size of hole and void density in mertenyl face.
（2）, porous graphene modified glassy carbon electrode obtain PG/GCE electrodes
By glass-carbon electrode（GCE）Successively with the α-Al of 1.0,0.3 and 0.05 M on chamois leather2O3The turbid liquid of powder makees polishing, connects
It is 1 deionized water, mass ratio successively:1 HNO3Respectively ultrasound 3min cleanings obtain clean glass-carbon electrode with acetone.Will
5.0mg PG are dispersed in 2.5mL high purity waters and ultrasound 30min, and PG dispersion liquid of the concentration for 2.0mg/mL is obtained.Next, with
Range is that the syringe of 5.0 L 5.0 L PG dispersant liquid drops is coated in the GCE surfaces that clean up and is dried under infrared lamp and obtains
Obtain PG/GCE electrodes.
（3）, using porous graphene modified glassy carbon electrode detection food in amaranth
Using PG/GCE as working electrode, used as reference electrode, platinum electrode is used as auxiliary electrode, composition three for saturated calomel electrode
Electrode system；The three-electrode system is initially positioned at containing 5.0 × 10-6mol·L-1The pH of amaranth is 7.0 BR
（Britton-Robinson）In buffer solution, the stirring enrichment 210s under open-circuit condition, after standing 10s, in 0.5V to 1.0V
Potential range in be scanned using cyclic voltammetry, record cyclic voltammetry curve, research amaranth on PG/GCE surfaces
Electrochemical behavior.Can be seen that and naked GCE and graphene modified glass-carbon electrode from accompanying drawing 2（G/GCE）Compare, amaranth is in PG/
Oxidation peak current on GCE electrodes obtains significantly enhancing.Further with square wave stripping voltammetry 0.5V to 1.0V's
The amaranth of scanning variable concentrations in potential range, the parameter setting of square wave voltammetry is as follows：Current potential increment is 4mV；Amplitude is
25mV；Frequency is 10Hz；Electrochemical workstation is Shanghai occasion China CHI 660D work stations.Record square wave volt-ampere curve（See accompanying drawing
3a）, and read the oxidation peak current value of amaranth；The data obtained Jing statistics after, the concentration with amaranth as abscissa, peak current
It is worth for vertical coordinate, 5.0 × 10-9mol/L~1.0×10-6Standard curve is drawn in the range of mol/L（See accompanying drawing 3b）, test limit
For 0.8 × 10-10Mol/L, it is I (A)=45.77 × C (M) -0.18 (linear to extrapolate the corresponding equation of linear regression of amaranth
Coefficient R=0.996), the equation can be used to determine the concentration of amaranth in actual sample.
（4）, actual sample detection
Commercially available red wine and cocktail sample need not be processed especially.Take 1.0mL red wines or cocktail sample is placed in 100mL volumetric flasks
In, it is settled to 100mL with the BR buffer solution that pH is 7.0；According to step（3）Identical electrochemical test method is that square wave is molten
Go out voltammetry to test testing sample solution, to obtain solution to be measured in amaranth oxidation peak current value, will be resulting
Current value substitution step（3）Calculated in the equation of linear regression for obtaining, drawn the dense of amaranth in detected sample
Degree.Measurement result shows：The oxidation peak current value of amaranth is respectively 2.23 A and 2.05 A in the red wine for measuring and cocktail.
Contain amaranth in institute's test sample product, peak point current is substituted into calibration curve equation and is calculated, finally draw red wine and cocktail
In the concentration of contained amaranth should be 3.2 gmL-1With 2.9 gmL-1。
Based on above-mentioned test result, it can be seen that the method for the present invention has carried out quick detection, the method pair to amaranth
Amaranth detection inspection range of linearity width, test limit is low, and sensitivity is high, simple to operate, can be in the samples such as red wine and cocktail
Amaranth carry out detecting accurate quantitative analyses.
In a word, the present invention is prepared for porous graphene using simple metal etching method, by the dispersion of porous graphene
Drop-coated is prepared for porous graphene modified glassy carbon electrode in glassy carbon electrode surface, because porous graphene has big specific surface
Product, high electric conductivity, strong absorbability and good mass transfer effect, experiment is using the porous graphene modified glassy carbon electrode to food
Amaranth in product is detected.The detection method of the present invention has sensitivity higher, and test limit is low, and method is easy and result
Accurate advantage.
Above-mentioned embodiment is merely to illustrate present disclosure, but this is not limitation of the present invention, this area
Person skilled, without departing from the scope of the invention, can also make corresponding adjustment and modification, therefore all
The technical scheme that the mode of equivalent or equivalent variations is formed belongs to protection scope of the present invention.
Claims (4)
1. a kind of method that utilization porous graphene detects amaranth in food, it is characterised in that：Comprise the steps：
（1）, porous graphene prepare：
Nitric acid nickel by powder is dissolved in deionized water, then under agitation graphite oxide GO solution is added to into above-mentioned nitre
In sour nickel solution, it is 10 to control GO with the mass ratio of Ni elements：1；After by above-mentioned mixed solution ultrasound, mixed solution is turned rapidly
In shift-in freeze dryer, in less than liquid nitrogen vacuum freezing 48h is used at a temperature of 0 DEG C, then by the powder for obtaining with 10 DEG C/
Min speed is heated to 800 DEG C in tube furnace from room temperature, and keeps 1h in the Ar atmosphere of flowing, has obtained black solid powder
End；Finally, after cleaning being carried out to the black powder for obtaining so that the hole of graphenic surface displays with dilute hydrochloric acid, spend from
Sub- water washing, vacuum drying is obtained porous graphene PG；
（2）, porous graphene modified glassy carbon electrode obtain PG/GCE electrodes
By glass-carbon electrode GCE with α-Al2O3The turbid liquid of powder makees polishing, then cleans up glass-carbon electrode；PG is dispersed in into height
In pure water and ultrasound, PG dispersion liquids are obtained, PG dispersant liquid drops are coated in the GCE surfaces that clean up and are dried under infrared lamp and obtained
Obtain PG/GCE electrodes；
（3）, using porous graphene modified glassy carbon electrode detection food in amaranth
Using PG/GCE as working electrode, used as reference electrode, platinum electrode is used as auxiliary electrode, composition three for saturated calomel electrode
Electrode system；The three-electrode system is initially positioned at containing 5.0 × 10-6mol·L-1The pH of amaranth be 7.0 BR buffering it is molten
In liquid, the stirring enrichment 210s under open-circuit condition after standing 10s, utilizes cyclic voltammetric in the potential range of 0.5V to 1.0V
Method is scanned, and records cyclic voltammetry curve, studies electrochemical behavior of the amaranth on PG/GCE surfaces, it is known that amaranth exists
Oxidation peak current on PG/GCE obtains significantly enhancing；Further with square wave stripping voltammetry 0.5V to 1.0V electricity
The amaranth of variable concentrations is scanned in the range of position, square wave volt-ampere curve is recorded, and reads the oxidation peak current value of amaranth；Gained
Jing after statistics, as abscissa, peak point current is vertical coordinate to the concentration with amaranth to data, 5.0 × 10-9mol/L~1.0×10-6Standard curve is drawn in the range of mol/L, detection is limited to 0.8 × 10-10Mol/L, extrapolates the corresponding linear regression side of amaranth
Journey is I (μ A)=45.77 × C (μM) -0.18, and the equation is used for determining the concentration of amaranth in actual sample；
（4）, actual sample detection
Take sample to be placed in volumetric flask, with the BR buffer solution constant volumes that pH is 7.0；According to step（3）Identical electrochemistry is surveyed
Method for testing is that square wave stripping voltammetry is tested testing sample solution, to obtain solution to be measured in amaranth oxidation peak electricity
Flow valuve, by resulting current value substitution step（3）Calculated in the equation of linear regression for obtaining, drawn detected sample
The concentration of middle amaranth.
2. the method that utilization porous graphene according to claim 1 detects amaranth in food, it is characterised in that：Step
（3）And step（4）In, the parameter setting of square wave stripping voltammetry is as follows：Current potential increment is 4mV；Amplitude is 25mV；Frequency is
10Hz。
3. a kind of preparation method of porous graphene material, it is characterised in that：Comprise the steps：Nitric acid nickel by powder is dissolved in
In deionized water, then graphite oxide GO solution is added in above-mentioned nickelous nitrate solution under agitation, controls GO and Ni
The mass ratio of element is 10：1；After by above-mentioned mixed solution ultrasound, mixed solution is transferred in freeze dryer rapidly, in low
At a temperature of 0 DEG C use liquid nitrogen vacuum freezing 48h, then by the powder for obtaining with 10 DEG C/min speed in tube furnace from room temperature
800 DEG C are heated to, and 1h is kept in the Ar atmosphere of flowing, obtained black solid powder；Finally, with dilute hydrochloric acid to obtaining
After black powder carries out cleaning so that the hole of graphenic surface is displayed, it is washed with deionized, is vacuum dried, is obtained many
Hole Graphene PG.
4. a kind of method that utilization porous graphene modified glassy carbon electrode obtains PG/GCE electrodes, it is characterised in that：Including as follows
Step：
（1）, porous graphene prepare：
Nitric acid nickel by powder is dissolved in deionized water, then under agitation graphite oxide GO solution is added to into above-mentioned nitre
In sour nickel solution, it is 10 to control GO with the mass ratio of Ni elements：1；After by above-mentioned mixed solution ultrasound, mixed solution is turned rapidly
In shift-in freeze dryer, in less than liquid nitrogen vacuum freezing 48h is used at a temperature of 0 DEG C, then by the powder for obtaining with 10 DEG C/
Min speed is heated to 800 DEG C in tube furnace from room temperature, and keeps 1h in the Ar atmosphere of flowing, has obtained black solid powder
End；Finally, after cleaning being carried out to the black powder for obtaining so that the hole of graphenic surface displays with dilute hydrochloric acid, spend from
Sub- water washing, vacuum drying is obtained porous graphene PG；
（2）, porous graphene modified glassy carbon electrode obtain PG/GCE electrodes
By glass-carbon electrode GCE with α-Al2O3The turbid liquid of powder makees polishing, then cleans up glass-carbon electrode；PG is dispersed in into height
In pure water and ultrasound, PG dispersion liquids are obtained, PG dispersant liquid drops are coated in the GCE surfaces that clean up and are dried under infrared lamp and obtained
Obtain PG/GCE electrodes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003057.0A CN106610400B (en) | 2017-01-04 | 2017-01-04 | Utilize the method for amaranth in porous graphene detection food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003057.0A CN106610400B (en) | 2017-01-04 | 2017-01-04 | Utilize the method for amaranth in porous graphene detection food |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106610400A true CN106610400A (en) | 2017-05-03 |
| CN106610400B CN106610400B (en) | 2019-06-28 |
Family
ID=58637005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710003057.0A Expired - Fee Related CN106610400B (en) | 2017-01-04 | 2017-01-04 | Utilize the method for amaranth in porous graphene detection food |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106610400B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827103A (en) * | 2017-12-07 | 2018-03-23 | 太原理工大学 | The preparation method and applications of N doping porous graphene |
| CN110487863A (en) * | 2019-09-02 | 2019-11-22 | 扬州大学 | A method of sunset yellow content is detected using graphitized carbon modified electrode |
| CN112240896A (en) * | 2020-03-30 | 2021-01-19 | 天津理工大学 | Composite carbon electrode and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778496A (en) * | 2012-08-15 | 2012-11-14 | 常州大学 | Method for measuring amaranth by utilizing expanded graphite paste electrode |
| CN103645236A (en) * | 2013-10-15 | 2014-03-19 | 南京医科大学 | Preparation method of magnetic control induced amaranth molecular targeted electrochemical sensing membrane |
| CN104649253A (en) * | 2013-11-18 | 2015-05-27 | 国家纳米科学中心 | Preparing methods of porous graphene and porous graphene film |
-
2017
- 2017-01-04 CN CN201710003057.0A patent/CN106610400B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778496A (en) * | 2012-08-15 | 2012-11-14 | 常州大学 | Method for measuring amaranth by utilizing expanded graphite paste electrode |
| CN103645236A (en) * | 2013-10-15 | 2014-03-19 | 南京医科大学 | Preparation method of magnetic control induced amaranth molecular targeted electrochemical sensing membrane |
| CN104649253A (en) * | 2013-11-18 | 2015-05-27 | 国家纳米科学中心 | Preparing methods of porous graphene and porous graphene film |
Non-Patent Citations (3)
| Title |
|---|
| MEILING WANG ET.AL.: "Sensitive determination of Amaranth in drinks by highly dispersed CNT in graphene oxide "water" with the aid of small amounts of ionic liquid", 《FOOD CHEMISTRY》 * |
| 曹海亮: "石墨烯基超级电容器电极材料的制备与电化学性能研究", 《中国优秀硕士学位论文全文数据库（电子期刊） 工程科技II辑》 * |
| 石文秀 等: "石墨烯修饰电极的研究及其电化学检测苋菜红", 《中国卫生检验杂志》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827103A (en) * | 2017-12-07 | 2018-03-23 | 太原理工大学 | The preparation method and applications of N doping porous graphene |
| CN110487863A (en) * | 2019-09-02 | 2019-11-22 | 扬州大学 | A method of sunset yellow content is detected using graphitized carbon modified electrode |
| CN112240896A (en) * | 2020-03-30 | 2021-01-19 | 天津理工大学 | Composite carbon electrode and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106610400B (en) | 2019-06-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108445057B (en) | Preparation and analysis method of electrochemical sensor for detecting heavy metal ions | |
| CN107064277B (en) | A kind of preparation method and application of electrochemical sensor | |
| Zhao et al. | Rapid and sensitive determination of tartrazine using a molecularly imprinted copolymer modified carbon electrode (MIP-PmDB/PoPD-GCE) | |
| CN104007155B (en) | A kind of for detecting electrochemical sensor of Trace Hg and its preparation method and application in water body | |
| CN106610400B (en) | Utilize the method for amaranth in porous graphene detection food | |
| CN105758917A (en) | Preparation and catalytic application of Nafion/horseradish peroxidase/tricobalt tetraoxide-graphene/ionic liquid carbon paste electrode | |
| Yang et al. | Electrochemical impedance immunosensor for sub-picogram level detection of bovine interferon gamma based on cylinder-shaped TiO2 nanorods | |
| CN102944598A (en) | Preparation method and application of cell based sensor based on electrochemical reduction graphite oxide/gold nanoparticle composite membrane | |
| CN106018506A (en) | Method for detecting lead ions by utilizing electrochemical sensor | |
| CN103558268A (en) | Method for electrochemically detecting concentration of glucose in whole blood through integrated paper based micro-fluidic apparatus | |
| CN106525947B (en) | The method for detecting solution Glutathione peptide concentration | |
| CN109001276A (en) | The building and application of electrochemical sensor based on COFs material | |
| CN106290512A (en) | Modified electrode and its preparation method and application | |
| CN108776160B (en) | Method that is a kind of while detecting bisphenol-A and bisphenol S | |
| CN106596697B (en) | The detection method of sunset yellow in food | |
| Zhao et al. | Reduced graphene oxide-modified screen-printed carbon (rGO-SPCE)-based disposable electrochemical sensor for sensitive and selective determination of ethyl carbamate | |
| Wu et al. | Sensitive and selective determination of dopamine by electrochemical sensor based on molecularly imprinted electropolymerization of o-phenylenediamine | |
| Taei et al. | New modified multiwalled carbon nanotubes paste electrode for electrocatalytic oxidation and determination of warfarin in biological and pharmaceutical samples | |
| CN104330452B (en) | A kind of screen printing electrode of soft material modification and preparation method and application | |
| CN106290540A (en) | A kind of method of orderly silicon nano hole road thin film/indium-tin oxide electrode Electrochemical Detection lead ion | |
| Han et al. | Electrochemical Behavior and Voltammetric Determination of Chloramphenicol and Doxycycline Using a Glassy Carbon Electrode Modified with Single‐walled Carbon Nanohorns | |
| CN108387631A (en) | A kind of graphene-supported cobalt acid nanosized nickel rods compound and its application | |
| CN106680355B (en) | Utilize the method for sunset yellow in carbon onion supporting Pt nano particle composite material detection food | |
| CN107014878B (en) | Preparation method and application of carbon nano material modified foam nickel electrode | |
| CN108107098A (en) | Based on WO3The method of alcoholic strength in/FTO photoelectric materials detection white wine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190628 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |