CN107843625A - A kind of pRGO ANSA/ metallic nanoparticles combination electrode material, combination electrode and its preparation method and application - Google Patents
A kind of pRGO ANSA/ metallic nanoparticles combination electrode material, combination electrode and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of pRGO ANSA/ metallic nanoparticles combination electrode material, combination electrode and its preparation method and application.The combination electrode material includes pRGO ANSA and metallic nanoparticle, and part redox graphene pRGO and the naphthalene sulfonic acids ANSA of 6 amino 2 mass ratio are 1 in the pRGO ANSA:2~2:1, pRGO mass fraction is 0.0025 ~ 0.02 % in the combination electrode material, and the particle diameter of the metallic sodium grain of rice is not more than 50 nm, and the metallic nanoparticle is coated on the surface of the pRGO ANSA.In combination electrode material provided by the invention, pRGO ANSA hybrid nano-materials have preferable dissolubility, highly dispersible, and specific surface area is big, and electronic conduction ability is strong, and biocompatibility is strong；It is meanwhile compound with the metallic nanoparticle with preferable electro catalytic activity so that the advantages of combination electrode material pRGO ANSA/ metallic nanoparticles finally given have specific surface area big, and electronic conduction ability is strong, and biocompatibility is strong, and electro catalytic activity is good.The combination electrode obtained using the combination electrode material, there is excellent sensitivity, selectivity is good, easy to use.
Description
Technical field
The invention belongs to electrochemical field, and in particular to a kind of pRGO-ANSA/ metallic nanoparticles combination electrode material, answer
Composite electrode and its preparation method and application.
Background technology
Fluoroquinolone antibacterial agent is one kind to gram-negative bacteria such as Pseudomonas aeruginosa, Escherichia coli, Salmonella and leaching
Coccus etc. is respectively provided with the antimicrobial of powerful bactericidal action.However, widely using with antibiotic, the drug resistance of bacterium etc. is asked
Topic becomes increasingly conspicuous, evidence suggests the residual of antibiotic in vivo can make it is bacterial resistance occurred；It is anti-intestines and stomach to be induced simultaneously
Should, headache, dizzy, vomiting heatstroke nervous system reaction, or even induce depressed symptom, its caused toxic side effect and bad shadow
Ring the concern for having enjoyed people.There are many countries to work it out the maximum residue limit of fluoroquinolone antibiotics at present
Regulation.Mainly include at present for the detection method of FQNS：High performance liquid chromatography tandem mass spectrum method, efficient liquid phase
Chromatography, capillary electrophoresis and fluorimetry etc..Although these methods have the spy of good selectivity and high sensitivity
Point, but organic solvent consumption to be but present big for these methods, instrument price is expensive, and complex operation, sample needs pre-treatment etc.
Tedious steps, and require high for analyzing the technical merit of tester.Therefore there is an urgent need to establish it is a kind of it is quick, sensitive,
Reagent consumption is few, can the operating method of on-line analysis determine the content analysis method of FQNS.
Electrochemical analysis method is that one kind directly carries out redox reaction by determinand in electrode surface, passes through electronics
Transfer chemical signal is changed into the form of electric signal and is detected, while this method has that clever lightness is high, analyze speed is fast,
The advantages that reagent consumes less, instrumentation is simple.
In order to improve the electronic conduction ability of modified electrode and electrochemical catalysis performance, in the preparation process of sensor,
With reference to new material relevant feature, using carbon nanomaterial and metallic nanoparticle modification in electrode surface.Modified electrode nanometer
Material is mainly included the carbon nanomaterial based on multi-walled carbon nanotube, graphene etc. and received with Jenner's grain of rice, nano grain of silver, platinum
Metal nano material based on the grain of rice, copper nanoparticle, palladium nanoparticle etc..It is big that these decorative materials are respectively provided with reference area, electronics
Conducting power is strong, the advantages that biocompatibility, can significantly improve the sensitivity of electrochemical sensor.
But conventional graphite alkene is not soluble in water and organic solvent, it is difficult to dispersed nano-modified material is obtained, and then
Limit its application on electrode modification and electrochemical analysis detection.
Therefore, develop that a kind of specific surface area is big, and electronic conduction ability is strong, it is compound that biocompatibility is strong and solubility property is good
Electrode material has important Research Significance and application value.
The content of the invention
The defects of it is an object of the invention to overcome carbon nano-composite material solubility property difference in the prior art, there is provided a kind of
Combination electrode material.Combination electrode material specific surface area provided by the invention is big, and electronic conduction ability is strong, and biocompatibility is strong,
Electro catalytic activity is good, and solubility property is good.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of pRGO-ANSA/ metallic nanoparticles combination electrode material, the combination electrode material include partial reduction graphite oxide
Alkene -6- amino -2- naphthalene sulfonic acids hybrid nano-material pRGO-ANSA and metallic nanoparticle, in the pRGO-ANSA pRGO with
ANSA mass ratio is 1:2~2:1, pRGO mass fraction is 0.0025 ~ 0.02 % in the combination electrode material, the gold
The particle diameter of category sodium rice grain is not more than 50 nm, and the metallic nanoparticle is coated on the surface of the pRGO-ANSA.
In combination electrode material provided by the invention, 6- amino -2- naphthalene sulfonic acids ANSA and partial reduction graphene oxide
The pRGO-ANSA hybrid nano-materials that pRGO is mixed to get have preferable dissolubility, highly dispersible, and specific surface area is big,
Electronic conduction ability is strong, and biocompatibility is strong；It is meanwhile compound with the metallic nanoparticle with preferable electro catalytic activity so that most
The combination electrode material pRGO-ANSA/ metallic nanoparticles obtained eventually have specific surface area big, and electronic conduction ability is strong, biofacies
The advantages of capacitive is strong, and electro catalytic activity is good.
Partial reduction graphene oxide pRGO of the present invention, it can be prepared first by the Hummer chemical methodes of routine
Graphene oxide is obtained, then utilizes hydrazine hydrate（98%, mass ratio）Reduction treatment is carried out to obtained graphene oxide dispersion
Obtain.
Preferably, the mass ratio of the pRGO and ANSA are 1:1.
Preferably, pRGO mass fraction is 0.0075 % in the combination electrode material.
Preferably, the metallic sodium grain of rice is Jenner's grain of rice, nano grain of silver, platinum nanoparticle, copper nanoparticle or palladium nanoparticle
In one kind.
Preferably, the particle diameter of the metallic sodium grain of rice is 10 nm.
A kind of combination electrode, it is the compound electric that above-mentioned pRGO-ANSA/ metallic nanoparticles are modified on basal electrode
Pole, the mass concentration of the basal electrode surface p RGO is 0.035 ~ 0.283mg/cm2。
The modified electrode obtained in combination electrode material modification to basal electrode had into excellent sensitivity, selectivity
It is good, it is easy to use.
Conventional basal electrode is used equally in this combination electrode.
Preferably, the basal electrode is carbon paste electrode, glass-carbon electrode, gold electrode, platinum electrode or Ti electrode.
The preparation method of above-mentioned combination electrode, the preparation method comprise the following steps：
S1：PRGO and ANSA are uniformly dispersed in a solvent, produce pRGO-ANSA hybrid nano-material dispersion liquids；Will be described point
Basal electrode surface is arrived in dispersion liquid modification；
S2：Metallic nanoparticle is deposited into the electrode surface that S1 is obtained by way of electro-deposition and produces the combination electrode.
PRGO-ANSA hybrid nano-material dispersion liquids can be repaiied by means such as drop coating, coating and the spin coatings of routine in S1
Adorn basal electrode surface.
It can be uniformly dispersed in S1 by the condition such as ultrasound pRGO and ANSA in water.
Electro-deposition mode in S2 is conventional electro-deposition method.
Preferably, pRGO mass concentration is 0.025 ~ 0.200 in pRGO-ANSA hybrid nano-materials dispersion liquid in S1
mg/mL。
ANSA and the poor pRGO hydridization of dissolubility can be formed to the pRGO-ANSA of high degree of dispersion.
Preferably, electro-deposition mode is in S2：By metallic nanoparticle be dispersed in acid solution mass concentration be 5.0 ~
20.0 mg/mL metallic nanoparticle solution, it will be deposited in the electrode insertion metallic nanoparticle solution obtained by S1.
The conventional acid solution of electro-deposition is used equally in the present invention, such as HCl solution, H2SO4Solution etc..
Preferably, acid solution is HCl solution in S2, it is further preferable that the concentration of the HCl solution is 0.15 mol/
L。
Application of the above-mentioned combination electrode in the quantitative electrochemical analysis detection of the content of FQNS is also at this
In the protection domain of invention.
Preferably, the FQNS is Ofloxacin, Lomefloxacin, Ciprofloxacin, Norfloxacin or training fluorine
Sha Xing.
Using combination electrode provided by the invention, content that can be by the electrochemical method of routine to FQNS
Carry out quantitative detection.
A kind of detection method of FQNS content, the detection method comprise the following steps：With electrochemistry work
It is electrochemical analytical instrument to make station, and the combination electrode forms three electrodes as working electrode with reference electrode and auxiliary electrode
System；Three-electrode system is placed in the solution of containing fluoroquinolones medicine, carries out Electrochemical Scanning, you can measure fluoquinolone
Class medicament contg.
Conventional reference electrode has Ag/AgCl electrodes, calomel electrode etc.；Conventional auxiliary electrode has platinum electrode etc..Electrification
Conventional selection can be carried out according to the characteristic of reference electrode by learning sweep parameter.
Preferably, the reference electrode is Ag/AgCl electrodes, and the auxiliary electrode is platinum electrode, the fluorine-containing quinoline promise
The solution of ketone medicine is the phosphate buffer that the concentration of FQNS is 0.1 mol/L, the phosphate-buffered
The pH of liquid is 4.0 ~ 7.5, and the scanning voltage is 0.2 ~ 1.3V, 0 ~ 5min of stand-by period.
Compared with prior art, the present invention has the advantages that：
In combination electrode material provided by the invention, pRGO-ANSA hybrid nano-materials have preferable dissolubility, can highly divide
Dissipate, and specific surface area is big, electronic conduction ability is strong, and biocompatibility is strong；Meanwhile received with the metal with preferable electro catalytic activity
The grain of rice is compound so that the combination electrode material pRGO-ANSA/ metallic nanoparticles finally given have that specific surface area is big, and electronics passes
It is strong to lead ability, the advantages of biocompatibility is strong, and electro catalytic activity is good.The combination electrode obtained using the combination electrode material, tool
There is excellent sensitivity, selectivity is good, easy to use.
Brief description of the drawings
Fig. 1 is the combination electrode schematic diagram and FQNS concentration mensuration schematic diagram that embodiment 1 provides；
Fig. 2 is the pRGO-ANSA hybrid nano-material phenograms that embodiment 1 provides；
The MWCNT-CPE/pRGO-ANSA/Au modified electrode bioassay standard product Norfloxacins that Fig. 3 provides for embodiment 1 show difference
Pulse Voltammetry figure；
Fig. 4 is that the MWCNT-CPE/pRGO-ANSA/Au modified electrodes that embodiment 1 provides determine showing for various concentrations Norfloxacin
Poor Pulse Voltammetry figure, wherein, figure a is that blood concentration norfloxacin scope is in 1.0 ~ 50.0 μM and oxidation peak current graph of a relation, figure b
Blood concentration norfloxacin scope is in 0.03 ~ 1.0 μM and oxidation peak current graph of a relation；
Fig. 5 is that the MWCNT-CPE/pRGO-ANSA/Au modified electrodes that embodiment 1 provides determine promise fluorine sand in Yunnan Baiyao Capsule
The differential pulse voltammetry voltammogram of star；
Fig. 6 is that the MWCNT-CPE/pRGO-ANSA/Au modified electrodes that embodiment 1 provides determine promise in Shi Yao groups Ou Yi medicine companies
The differential pulse voltammetry voltammogram of Flucloxacillin；
After Fig. 7 is MWCNT-CPE/pRGO-ANSA/Au modified electrodes measure administration Norfloxacin 90 min that embodiment 1 provides
The differential pulse voltammetry voltammogram of medicine in SD rat bodies.
Embodiment
The present invention is expanded on further with reference to embodiment.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.The experimental method of unreceipted actual conditions in lower example embodiment, generally according to this area normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw material and reagent that approach obtains.The change for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replace and belong to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of pRGO-ANSA/ metallic nanoparticles combination electrode material, and the combination electrode material includes part also
Former graphene oxide -6- amino -2- naphthalene sulfonic acids hybrid nano-material pRGO-ANSA and Jenner grain of rice Au, wherein, pRGO-ANSA
Middle pRGO and ANSA mass ratio are 1:1, pRGO mass fraction is 0.0075 % in combination electrode material, the golden sodium rice grain
Particle diameter be 10 nm, Jenner's grain of rice is coated on the surface of the pRGO-ANSA.
Using the pRGO-ANSA that the present embodiment provides as decorative material, multi-walled carbon nanotube carbon paste electrode is filled（MWCNT-
CPE）As basal electrode, modified using electrochemical deposition Au nanoparticles to electrode surface and obtain MWCNT-CPE/pRGO-ANSA/
Au combination electrodes, specific preparation process are as follows：
Weigh 300 mg multi-walled carbon nanotubes and 700 mg graphite powders are put into that 40 μ L atoleines are added into agate mortar is abundant
Grinding is uniform, grinding in the uniform carbon paste PTFE tube that filling is 3 mm to internal diameter by hand, the mm of depth of cracking closure about 3, is inside inserted with
Carbon paste in PTFE tube is compacted as conductor, the carbon paste electrode surface of compacting is polished on pan paper by adjustable copper post
Into plane.Take 0.075 mg/mL partial reductions graphene oxide and 6- amino -2- naphthalene sulfonic acids dispersion liquid (1:1, m/m) 10 μ
L drop coatings are to MWCNT-CPE electrode surfaces, naturally dry at ambient temperature, you can the MWCNT-CPE/pRGO- modified
ANSA.PRGO-ANSA/MWCNTs-CPE electrodes are inserted into by 10.0 mg/mL using electrochemistry i-t patterns again（Containing 0.15
mol/L HCl）Jenner's grain of rice（Particle diameter is 10 nm）In solution, under the conditions of -0.9 V, 0.5 min is deposited, you can repaiied
Adorn the multi-walled carbon nanotube carbon paste electrode of electrode pRGO-ANSA/Au modifications（Such as Fig. 1）.
（1）PRGO-ANSA hybrid nano-materials characterize
Table is carried out to the pRGO-ANSA hybrid nano-materials of formation using the type ultraviolet-visible-near-infrared spectrum instrument of Lambda 950
Sign.There are two characteristic absorption peaks at 234 nm and 296 nm for graphene oxide, wherein 234 nm are due to C=C π-π *
Conjugation is formed, and the absworption peak at 296 nm is due to that C=O n- π * are conjugated to be formed.After graphene oxide is by hydrazine hydrate reduction
Its absworption peak significantly reduces, and the peak red shift of 234 nm absorption is to 250 nm, while 296 nm acromion disappears.For 6- ammonia
Base -2- naphthalene sulfonic acids has a strong absworption peak at 242 nm.The pRGO-ANSA hybrid nano-materials of formation, the suction of graphene
Receive peak difference red shift to 286 and 330 nm, the absworption peak red shift of 6- amino -2- naphthalene sulfonic acids and show that pRGO-ANSA is miscellaneous to 254 nm
Change nano material and carry out good hydridization.It is can be found that simultaneously by Fig. 2 compared with the graphene oxide of partial reduction,
PRGO-ANSA hybrid nano-materials have more preferable dispersive property（Such as Fig. 2）.
（2）The assay of standard items Norfloxacin
Using electrochemical workstation as experimental analysis instrument, respectively using Ag/AgCl as reference electrode, platinum electrode is auxiliary electrode,
The MWCNT-CPE/pRGO-ANSA/Au that the present embodiment provides is working electrode, the three-electrode system of composition；In 0.2 ~ 1.3 V
（vs. Ag/AgCl）Differential pulse voltammetry voltammetric scan is carried out in potential range, records stable differential pulse voltammetry voltammogram（Such as Fig. 3）：
Modified electrode presents in the range of 0.03 ~ 1.0 μm of ol/L and 1.0 ~ 50.0 μm of ol/L good linear respectively to Norfloxacin
Relation, detection are limited to 0.016 μm of ol/L（S/N=3）, linear equation is：Ip=0.139CNFX+0.356 (R2=0.9994, concentration
1.0 ~ 50.0 μm of ol/L and Ip=0.381C of scopeNFX+0.170 (R2=0.9903,0.03 ~ 1.0 μm of ol/L of concentration range)
(Ip oxidation peak currents, μ A；CNFXBlood concentration norfloxacin, mol/L)（Such as Fig. 4）.
（3）The assay of Norfloxacin in Yunnan Baiyao Capsule
The content of Norfloxacin in Yunnan Baiyao Capsule is measured according to standard items Norfloxacin identical method of testing, its
Differential pulse voltammetry voltammogram such as Fig. 5.As seen from the figure, using the present embodiment provide combination electrode can quickly, sensitively to the medicine
In the content of Norfloxacin detected.
（4）The assay of Norfloxacin in Shi Yao groups Ou Yi medicine companies
The content of Norfloxacin in Shi Yao groups Ou Yi medicine companies is surveyed according to standard items Norfloxacin identical method of testing
It is fixed, its differential pulse voltammetry voltammogram such as Fig. 6.As seen from the figure, using the present embodiment provide combination electrode can quickly, sensitively to this
The content of Norfloxacin in medicine is detected.
（5）The assay of medicine in SD rat bodies after Norfloxacin 90 min is administered
Medicine in SD rat bodies after the administration min of Norfloxacin 90 is contained according to standard items Norfloxacin identical method of testing
Amount is measured, its differential pulse voltammetry voltammogram such as Fig. 7.As seen from the figure, the combination electrode provided using the present embodiment can quickly, it is clever
The quick content to the Norfloxacin in the medicine detects.
Embodiment 2
The present embodiment provides a kind of pRGO-ANSA/ Jenners grain of rice combination electrode material, and the combination electrode material includes partial reduction
Graphene oxide -6- amino -2- naphthalene sulfonic acids hybrid nano-material pRGO-ANSA and Jenner grain of rice Au, wherein, in pRGO-ANSA
PRGO and ANSA mass ratio is 1:1, pRGO mass fraction is 0.02 % in combination electrode material, the grain of the golden sodium rice grain
Footpath is 10 nm, and Jenner's grain of rice is coated on the surface of the pRGO-ANSA.
Using the pRGO-ANSA that the present embodiment provides as decorative material, using MWCNT-CPE electrodes as basal electrode, use
The modification of electrochemical deposition Au nanoparticles obtains MWCNT-CPE/pRGO-ANSA/Au combination electrodes to electrode surface, specific to prepare step
It is rapid as follows：
The preparation method of carbon paste electrode is consistent with embodiment 1.Weigh 0.200 mg/mL partial reductions graphene oxide and 6-
Amino -2- naphthalene sulfonic acids dispersion liquid (1:1, m/m) 10 μ L drop coatings are natural at ambient temperature to MWCNT-CPE electrode surfaces
Dry, you can the MWCNT-CPE/pRGO-ANSA modified.Electrochemistry i-t patterns are used again by pRGO-ANSA/MWCNTs-
CPE electrodes are inserted into 5.0 mg/mL（Containing 0.15 mol/L HCl）Jenner's grain of rice（Particle diameter is 10 nm）In solution ,-
Under the conditions of 0.9 V, 3 min are deposited, you can obtain the multi-walled carbon nanotube carbon paste electrode of modified electrode pRGO-ANSA/Au modifications.
The Au/pRGO-ANSA/Pt combination electrodes of embodiment 3
The present embodiment provides a kind of pRGO-ANSA/ metallic nanoparticles combination electrode material, and the combination electrode material includes part also
Former graphene oxide -6- amino -2- naphthalene sulfonic acids hybrid nano-material pRGO-ANSA and platinum nanoparticle Pt, wherein, pRGO-ANSA
Middle pRGO and ANSA mass ratio are 2:1, pRGO mass fraction is 0.0025 % in combination electrode material, the platinum sodium rice grain
Particle diameter be 5 nm, the platinum nanoparticle is coated on the surface of the pRGO-ANSA.
Using the pRGO-ANSA that the present embodiment provides as decorative material, using Au electrodes as basal electrode, a diameter of 3 mm,
Modified using electrochemical deposition Pt nanoparticles to electrode surface and obtain Au/pRGO-ANSA/Pt combination electrodes, specific preparation process
It is as follows：
Take 0.025 mg/mL partial reductions graphene oxide and 6- amino -2- naphthalene sulfonic acids dispersion liquid (2:1, m/m) 10 μ L drops
Au electrode surfaces are coated onto, at ambient temperature naturally dry, you can the Au/pRGO-ANSA modified.Electrochemistry i- is used again
PRGO-ANSA/Au electrodes are inserted into 20.0 mg/mL by t patterns（Containing 0.15 mol/L HCl）Pt nanoparticles（Particle diameter is 5
nm）In solution, under the conditions of -0.3 V, 1 min is deposited, you can obtain modified electrode Au/pRGO-ANSA/Pt.
The Pt/pRGO-ANSA/Pd combination electrodes of embodiment 4
The present embodiment provides a kind of pRGO-ANSA/ metallic nanoparticles combination electrode material, and the combination electrode material includes part also
Former graphene oxide -6- amino -2- naphthalene sulfonic acids hybrid nano-material pRGO-ANSA and palladium nanoparticle Pd, wherein, pRGO-ANSA
Middle pRGO and ANSA mass ratio are 1:2, pRGO mass fraction is 0.01% in combination electrode material, the palladium sodium rice grain
Particle diameter is 30 nm, and the palladium nanoparticle is coated on the surface of the pRGO-ANSA.
Using the pRGO-ANSA that the present embodiment provides as decorative material, using Pt electrodes as basal electrode, a diameter of 3 mm,
Modified using electrochemical deposition Pd nanoparticles to electrode surface and obtain Pt/pRGO-ANSA/Pd combination electrodes, specific preparation process
It is as follows：
Take 0.100 mg/mL partial reductions graphene oxide and 6- amino -2- naphthalene sulfonic acids dispersion liquid (1:2, m/m) 10 μ L drops
Pt electrode surfaces are coated onto, at ambient temperature naturally dry, you can the Pt/pRGO-ANSA modified.Electrochemistry i- is used again
Pt/pRGO-ANSA electrodes are inserted into 20.0 mg/mL by t patterns（Containing 0.15 mol/L HCl）Pd nanoparticles（Particle diameter is 30
nm）In solution, under the conditions of -1.2 V, 2 min are deposited, you can obtain modified electrode Pt/pRGO-ANSA/Pd.
Claims (10)
1. a kind of pRGO-ANSA/ metallic nanoparticles combination electrode material, it is characterised in that the combination electrode material includes portion
Divide redox graphene -6- amino -2- naphthalene sulfonic acids hybrid nano-material pRGO-ANSA and metallic nanoparticle, the pRGO-
PRGO and ANSA mass ratio is 1 in ANSA:2~2:1, in the combination electrode material pRGO mass fraction for 0.0025 ~
0.02%, the particle diameter of the metallic sodium grain of rice is not more than 50 nm, and the metallic nanoparticle is coated on the table of the pRGO-ANSA
Face.
2. pRGO-ANSA/ metallic nanoparticles combination electrode material according to claim 1, it is characterised in that the pRGO and
ANSA mass ratio is 1:1.
3. pRGO-ANSA/ metallic nanoparticles combination electrode material according to claim 1, it is characterised in that the compound electric
PRGO mass fraction is 0.0075 % in the material of pole.
4. pRGO-ANSA/ metallic nanoparticles combination electrode material according to claim 1, it is characterised in that the metallic sodium
The particle diameter of the grain of rice is 10 nm.
5. a kind of combination electrode, it is characterised in that any pRGO-ANSA/ gold of claim 1 ~ 4 is modified on basal electrode
Category nanoparticle produces the combination electrode, and the mass concentration of the basal electrode surface p RGO is 0.035 ~ 0.283 mg/cm2。
6. the preparation method of combination electrode described in a kind of claim 5, it is characterised in that the preparation method includes following step
Suddenly：
S1：PRGO and ANSA are uniformly dispersed in a solvent, produce pRGO-ANSA hybrid nano-material dispersion liquids；Will be described point
Basal electrode surface is arrived in dispersion liquid modification；
S2：Metallic nanoparticle is deposited into the electrode surface that S1 obtains by electro-deposition mode and produces the combination electrode.
7. the preparation method of combination electrode according to claim 6, it is characterised in that pRGO-ANSA hybridized nanometers material in S1
The mass concentration for expecting pRGO in dispersion liquid is 0.025 ~ 0.200 mg/mL.
8. the preparation method of combination electrode according to claim 6, it is characterised in that electro-deposition mode is in S2：By metal
Nanoparticle is dispersed to the metallic nanoparticle solution for obtaining that mass concentration is 5.0 ~ 20.0 mg/mL in acid solution, by the electricity obtained by S1
Pole is inserted in the metallic nanoparticle solution and deposited.
A kind of 9. quantitative electrochemical analysis detection of content of combination electrode according to claim 5 in FQNS
In application.
10. apply according to claim 9, it is characterised in that the FQNS is Ofloxacin, Lome sand
Star, Ciprofloxacin, Norfloxacin or Pefloxacin.
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