CN106610400B - Utilize the method for amaranth in porous graphene detection food - Google Patents
Utilize the method for amaranth in porous graphene detection food Download PDFInfo
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- 235000012735 amaranth Nutrition 0.000 title claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 41
- 238000001514 detection method Methods 0.000 title claims abstract description 24
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- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 4
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- 238000007254 oxidation reaction Methods 0.000 claims description 10
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- 229910052799 carbon Inorganic materials 0.000 claims description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 6
- 238000002484 cyclic voltammetry Methods 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
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- 238000013019 agitation Methods 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 5
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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 present invention relates to a kind of methods using amaranth in porous graphene detection food, belong to analytical chemistry field or field of food safety.The present invention is prepared for porous graphene using simple metal etching method, the dispersant liquid drop of porous graphene is coated in glassy carbon electrode surface and is prepared for porous graphene modified glassy carbon electrode, since porous graphene has big specific surface area, high electric conductivity, strong adsorption capacity and good mass transfer effect, experiment detect the amaranth in food using the porous graphene modified glassy carbon electrode.Detection method of the invention has sensitivity higher, and detection limit is low, method simplicity and the accurate advantage of result.
Description
Technical field
The present invention relates to electrochemical 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 technique
Using the development of Electrochemical Detection food additives, drug and biomolecule cause a series of biosensors,
The quick appearance of food sensing and environmental sensor.Since its high sensitivity, price are low high, easy to operate and be easy small-sized
The advantages that change, electrochemical measuring technique have been successfully applied to protein analysis, biological monitoring, Pharmaceutical Analysis and food point
The fields such as analysis.In order to cause everybody appetite, the pigments such as amaranth are often added in the food such as dessert, candy, beverage.Root
It is provided according to food hygiene tissue (FAO) and the World Health Organization (WHO), 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 is often added to excessive amaranth in product.
Therefore, it realizes 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.
Summary of the invention
Based on the above-mentioned prior art, detected the object of the present invention is to provide a kind of using porous graphene modified glassy carbon electrode
The method of amaranth.It is prepared for porous graphene modified glassy carbon electrode sensor using metal etching method, utilizes porous graphite
The big specific surface area of alkene and fabulous mass transfer effect have carried out quick detection to the amaranth in food.
The present invention is achieved by the following technical scheme:
A method of using amaranth in porous graphene detection food, include the following steps:
(1), prepared by porous graphene
Nitric acid nickel by powder is dissolved in deionized water, then graphite oxide GO solution is added under agitation on
It states in nickel nitrate solution, the mass ratio of control GO and Ni element is 10:1；After above-mentioned mixed solution ultrasound, it will mix rapidly molten
Liquid is transferred into freeze-dryer, liquid nitrogen vacuum refrigeration 48h is used at a temperature of lower than 0 DEG C, then by obtained powder with 10
DEG C/min rate is heated to 800 DEG C from room temperature in tube furnace, and keeps 1h in the Ar atmosphere of flowing, obtain black solid
Powder；Finally, being spent after being cleaned to obtained black powder with dilute hydrochloric acid so that the hole of graphene surface displays
Porous graphene PG is made in ion water washing, vacuum drying.
(2), porous graphene modified glassy carbon electrode PG/GCE
By glass-carbon electrode GCE α-Al2O3Powder turbid makees polishing treatment, then cleans up glass-carbon electrode；PG is dispersed in
In high purity water and PG dispersant liquid drop is coated in the surface GCE cleaned up and dried under infrared lamp by ultrasound, obtained PG dispersion liquid
Obtain electrode PG/GCE.
(3), amaranth in porous graphene modified glassy carbon electrode detection food is utilized
Using PG/GCE as working electrode, saturated calomel electrode is as reference electrode, and platinum electrode is as auxiliary electrode, group
At three-electrode system；The three-electrode system is initially positioned at containing 5.0 × 10-6mol·L-1The BR that the pH of amaranth is 7.0 is slow
It rushes in solution, the stirring enrichment 210s under open-circuit condition after standing 10s, utilizes circulation in the potential range of 0.5V to 1.0V
Voltammetry is scanned, and records cyclic voltammetry curve, electrochemical behavior of the research amaranth on the surface PG/GCE, it is known that amaranth
Oxidation peak current on PG/GCE obtains apparent enhancing；Further using square wave stripping voltammetry 0.5V to 1.0V's
The amaranth of scanning various concentration, the parameter setting of square wave voltammetry are as follows in potential range: current potential increment is 4mV；Amplitude is
25mV；Frequency is 10Hz；Square wave volt-ampere curve is recorded, and reads the oxidation peak current value of amaranth；The data obtained after counting,
Using the concentration of amaranth as abscissa, peak point current is ordinate, 5.0 × 10-9mol/L~1.0×10-6Within the scope 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 be I (μ A)=
45.77 × C (μM) -0.18, the equation are used to measure the concentration of amaranth in actual sample.
(4), actual sample detects
Sample is taken to be placed in volumetric flask, the BR buffer solution constant volume for being 7.0 with pH；According to electrification identical with step (3)
It learns test method, that is, square wave stripping voltammetry to test testing sample solution, to obtain the oxidation of amaranth in solution to be measured
Peak point current will be calculated in equation of linear regression that obtained current value substitution is obtained with step (3), be obtained to be detected
The concentration of amaranth in sample.
The porous graphene synthesized in the present invention has the hole of nano-scale, and hole is uniform, and this structure makes this
When porous graphene is as electrode material, not only there is big specific surface area, while there are also good mass transfer effects, it 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 this method detection effect is more preferable, and detection limit is lower and easy to operate, time saving,
It has a extensive future.
Detailed description of the invention
Fig. 1 shows the TEM of porous graphene of the present invention figures.
Fig. 2 indicates that GCE electrode (b), G/GCE electrode (c) and PG/GCE electrode (d) are including 5.0 × 10-6mol·L-1Amaranth
The red 0.1molL of dish-1PH be 7.0 BR buffer solution in cyclic voltammogram；Indicate that PG/GCE electrode (a) is not including
The 0.1molL of amaranth-1PH be 7.0 BR buffer solution in cyclic voltammogram, scanning speed 100mVs-1。
Fig. 3 a indicates square wave voltammogram of the amaranth of various concentration in the present invention on PG/GCE electrode.
Fig. 3 b indicates that in the present invention by abscissa, peak point current of amaranth concentration be the linear relationship chart of ordinate.
Specific embodiment
A specific embodiment of the invention is further illustrated below.
A method of using amaranth in porous graphene detection food, include the following steps:
(1), prepared by porous graphene
A certain amount of nickel nitrate (II) powder is dissolved in 15mL deionized water, it is then under agitation that 10mL is dense
Degree is 4mgmL -1Graphite oxide (GO) solution be added in above-mentioned nickelous nitrate solution.Control the mass ratio of GO and Ni element
For 10:1.After above-mentioned mixed solution ultrasound 10min, mixed solution is transferred into freeze-dryer rapidly, in lower than 0 DEG C
At a temperature of use liquid nitrogen vacuum refrigeration 48h, then obtained powder is heated in tube furnace from room temperature with 10 DEG C/min rate
800 DEG C, and 1h is kept in the Ar atmosphere of flowing, obtain black solid powder.Finally, with dilute hydrochloric acid to obtained black powder
It after end is cleaned so that the hole of graphene surface displays, is washed with a large amount of deionized waters, is dried in vacuo, is made porous
Graphene (PG).The TEM that attached drawing 1 is PG schemes, can be porous to adjust by adjusting the mass ratio of GO and Ni in this preparation method
The size of hole and void density in graphene basal plane.
(2), porous graphene modified glassy carbon electrode obtains PG/GCE electrode
By glass-carbon electrode (GCE) successively with 1.0,0.3 and 0.05 μM of α-Al on chamois leather2O3Powder turbid makees polishing treatment,
Then the HNO for being successively 1:1 with deionized water, mass ratio3Ultrasound 3min cleaning obtains clean glass-carbon electrode respectively with acetone.
5.0mg PG is dispersed in 2.5mL high purity water simultaneously ultrasound 30min, the PG dispersion liquid that concentration is 2.0mg/mL is made.Next,
5.0 μ L PG dispersant liquid drops are coated in the surface GCE cleaned up with the syringe that range is 5.0 μ L and are dried under infrared lamp
Obtain PG/GCE electrode.
(3), amaranth in porous graphene modified glassy carbon electrode detection food is utilized
Using PG/GCE as working electrode, saturated calomel electrode is as reference electrode, and platinum electrode is as auxiliary electrode, group
At three-electrode system；The three-electrode system is initially positioned at containing 5.0 × 10-6mol·L-1The BR that the pH of amaranth is 7.0
(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, study amaranth on the surface PG/GCE
Electrochemical behavior.From attached drawing 2 as can be seen that compared with naked GCE and graphene modified glass-carbon electrode (G/GCE), amaranth is in PG/
Oxidation peak current on GCE electrode obtains apparent enhancing.Further using square wave stripping voltammetry 0.5V to 1.0V's
The amaranth of scanning various concentration, the parameter setting of square wave voltammetry are as follows in potential range: current potential increment is 4mV；Amplitude is
25mV；Frequency is 10Hz；Electrochemical workstation is Shanghai Chen Hua CHI 660D work station.Square wave volt-ampere curve is recorded (see attached drawing
3a), and the oxidation peak current value of amaranth is read；The data obtained is after counting, using the concentration of amaranth as abscissa, peak current
Value is ordinate, 5.0 × 10-9mol/L~1.0×10-6Standard curve (see attached drawing 3b) is drawn within the scope of mol/L, detection limit
It is 0.8 × 10-10Mol/L, extrapolating the corresponding equation of linear regression of amaranth is I (μ A)=45.77 × C (μM) -0.18 (linear
Coefficient R=0.996), the equation can be used to measure the concentration of amaranth in actual sample.
(4), actual sample detects
Commercially available red wine and cocktail sample need not be handled especially.1.0mL red wine or cocktail sample is taken to be placed in 100mL capacity
In bottle, 100mL is settled to the BR buffer solution that pH is 7.0；According to electrochemical test method, that is, square wave identical with step (3)
Stripping voltammetry tests testing sample solution, to obtain the oxidation peak current value of amaranth in solution to be measured, by gained
To the equation of linear regression that is obtained with step (3) of current value substitution in calculated, obtain amaranth in sample to be tested
Concentration.Measurement result shows: the oxidation peak current value of amaranth is respectively 2.23 μ A and 2.05 μ in the red wine and cocktail measured
A.Contain amaranth in institute's sample, peak point current is substituted into calibration curve equation and is calculated, finally obtains red wine and chicken tail
The concentration of amaranth contained in wine should be 3.2 μ gmL-1With 2.9 μ gmL-1。
Based on above-mentioned test result, it can be seen that method of the invention has carried out quick detection, this method pair to amaranth
The amaranth detection inspection range of linearity is wide, and detection limits low, high sensitivity, easy to operate, can be in the samples such as red wine and cocktail
Amaranth carry out detecting accurate quantitative analysis.
In short, 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, since porous graphene has big specific surface
Product, high electric conductivity, strong adsorption capacity and good mass transfer effect, experiment is using the porous graphene modified glassy carbon electrode to food
Amaranth in product is detected.Detection method of the invention has sensitivity higher, and detection limit is low, method simplicity and result
Accurate advantage.
Above embodiment is merely to illustrate the contents of the present invention, but this is not a limitation of the present invention, this field
Related technical personnel can also make corresponding adjustment and modification, therefore all without departing from the scope of the invention
The technical solution that the mode of equivalent replacement or equivalent variations is formed all belongs to the scope of protection of the present invention.
Claims (1)
1. a kind of method using amaranth in porous graphene detection food, characterized by the following steps:
(1), prepared by porous graphene:
Nitric acid nickel by powder is dissolved in deionized water, graphite oxide GO solution is then added to above-mentioned nitre under agitation
In sour nickel solution, the mass ratio of control GO and Ni element is 10:1；After above-mentioned mixed solution ultrasound, mixed solution is turned rapidly
Be moved into freeze-dryer, in lower than liquid nitrogen vacuum refrigeration 48h is used at a temperature of 0 DEG C, then by obtained powder with 10 DEG C/
Min rate is heated to 800 DEG C from room temperature in tube furnace, and keeps 1h in the Ar atmosphere of flowing, has obtained black solid powder
End；Finally, after being cleaned to obtained black powder with dilute hydrochloric acid so that the hole of graphene surface displays, spend from
Porous graphene PG is made in sub- water washing, vacuum drying；
(2), porous graphene modified glassy carbon electrode obtains PG/GCE electrode
By glass-carbon electrode GCE with α-Al2O3Powder turbid makees polishing treatment, then cleans up glass-carbon electrode；PG is dispersed in height
In pure water and PG dispersant liquid drop is coated in the surface GCE cleaned up and dried under infrared lamp and obtained by ultrasound, obtained PG dispersion liquid
Obtain PG/GCE electrode；
(3), amaranth in porous graphene modified glassy carbon electrode detection food is utilized
Using PG/GCE as working electrode, saturated calomel electrode is as reference electrode, and platinum electrode is as auxiliary electrode, composition three
Electrode system；The three-electrode system is initially positioned at containing 5.0 × 10-6mol·L-1The BR buffering that the pH of amaranth is 7.0 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, electrochemical behavior of the research amaranth on the surface PG/GCE, it is known that amaranth exists
Oxidation peak current on PG/GCE obtains apparent enhancing；Further utilize square wave stripping voltammetry in the electricity of 0.5V to 1.0V
The amaranth of scanning various concentration, records square wave volt-ampere curve, and read the oxidation peak current value of amaranth in the range of position；Gained
Data are after counting, and using the concentration of amaranth as abscissa, peak point current is ordinate, 5.0 × 10-9mol/L~1.0×10-6Standard curve is drawn within the scope 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 to measure the concentration of amaranth in actual sample；
(4), actual sample detects
Sample is taken to be placed in volumetric flask, the BR buffer solution constant volume for being 7.0 with pH；It is surveyed according to electrochemistry identical with step (3)
Method for testing, that is, square wave stripping voltammetry tests testing sample solution, to obtain the oxidation peak electricity of amaranth in solution to be measured
Flow valuve will calculate in equation of linear regression that obtained current value substitution is obtained with step (3), obtain sample to be tested
The concentration of middle amaranth；
In step (3) and step (4), the parameter setting of square wave stripping voltammetry is as follows: current potential increment is 4mV；Amplitude is 25mV；
Frequency is 10Hz.
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| 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 |
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| CN102778496A (en) * | 2012-08-15 | 2012-11-14 | 常州大学 | Method for measuring amaranth by utilizing expanded graphite paste electrode |
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| 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 |
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