CN106248766B - A kind of application of electrochemical sensor in measurement drug in paracetamol content - Google Patents
A kind of application of electrochemical sensor in measurement drug in paracetamol content Download PDFInfo
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Abstract
The present invention relates to material preparations and Electroanalytical Chemistry technical field, and in particular to a kind of CoFe2O4NWs/RGO nanocomposite and its paracetamol electrochemical sensor being prepared.The nanocomposite comprises the following steps: graphene oxide (GO) is first placed in water 10~30min of ultrasound by S11., and citric acid is then added and continues 10~60min of ultrasound, obtains graphene oxide (GO) dispersion liquid；S12. by FeCl3·6H2O and CoCl2·6H2O is added in graphene oxide (GO) dispersion liquid, is ultrasonically treated 10~60min；S13. pH value is adjusted to 9.5~10.5, and hydrazine is added, stirs 30~120min, is aged 18~48h；S14. it is centrifuged, washs, obtains CoFe after drying2O4NWs/RGO nanocomposite.The chemical electrode or electrochemical sensor being prepared with the nanocomposite have the advantages that stability is good, detection limit is low, sensitivity and selectivity are high during measuring paracetamol.
Description
Technical field
The present invention relates to material preparations and Electroanalytical Chemistry technical field, and in particular to a kind of CoFe2O4NWs/RGO nanometers
Composite material and its paracetamol electrochemical sensor being prepared.
Background technique
Paracetamol, the entitled acamol of chemistry, it belongs to the acetophenone amine in organic compound, is a kind of
Common analgesic-antipyretic.The physiological action principle of paracetamol is the release of main control Cycloxygenase, and then inhibits inferior colliculus
The synthesis of brain heat-regulating centers prostaglandin makes human peripheral blood pipe constantly uphold, perspire and achievees the effect that antipyretic, solution
The effect of hot throe can be similar to aspirin, to slight, moderate pain is effective.Therefore, paracetamol to treatment or is alleviated
Cat fever, arthralgia, neuralgia, migraine, toothache and postoperative pain etc. have certain curative effect.Long-term or excessive use is flutterred
Heat breath pain, can damage human organ, or even can inhibit the respiratory center of human body, show anorexia, nausea, abdominal pain
Etc. symptoms, it is also possible to there is hepatonecrosis.The main reason is that the primary product that hydrolysis occurs for paracetamol is to amino
Phenol, the substance have toxicity, human organ can be caused to be poisoned.Therefore, developing a kind of can rapidly and accurately detect paracetamol
Analysis method, for instructing clinical application to be of great significance safely.
Method currently used for detecting paracetamol mainly has spectrophotometry, liquid chromatography, Capillary Electrophoresis, chemistry
Luminescence method and Capillary Electrophoresis-ultraviolet spectroscopy etc..But there is required equipment price valuableness, sample are pre- for most of these methods
The problems such as complicated, cumbersome, time-consuming is handled, the requirement of clinical detection cannot be met very well.For solve it is above-mentioned there is
Problem, the present invention provide a kind of high sensitivity, easy to operate, low in cost, response quickly, can real-time detection electrochemical method
Quantitative detection for paracetamol.This is because paracetamol belongs to the antifebrin substance in organic acid, there is amide
With the structure of phenol, hydroxyl and amino in the structure can provide hydrogen ion, and hydrogen ion has stronger oxidisability, this makes
It is possibly realized using electrochemical method determining paracetamol.
It is in the majority with probing into for modified electrode in the report of electrochemical method determining paracetamol, this is because bare electrode
Electro catalytic activity it is low, it is weak to the electrochemical response of analyte.Functional nanocomposite is with polynary nanometer material by multiple
The heterogeneous material for closing technique and preparing, a variety of materials make up for each other's deficiencies and learn from each other in performance, generate synergistic effect, make composite material
Comprehensive performance is better than former composition material.In electrode modified material field, nanocomposite is typically exhibited better than one pack system
The electro catalytic activity of material, to greatly improve sensitivity and the detection limit of electrochemical sensor.Currently, report is flutterred for enhancing
The electrode modified material of heat breath pain electrochemical response signal is concentrated mainly on the Complex Function to carbon nanotube, such as chitosan-
Cu/ carbon nanotube (Mao A, Li H, Jin D, Yu L, Hu X, Talanta 144 (2015) 252-257), Cu-C60/ carbon is received
Mitron (Brahman P K, Suresh L, Lokesh V, Nizamuddin S, Analytica Chimica Acta, 917
(2016)107–116)、 WO3/ carbon nanotube (Baytak A K, Duzmen S, Teker T, Aslanoglu M,
Materials Science and Engineering:C 57 (2015) 164-170) etc.；But these function nano composite woods
Expect that film forming is poor so that there is the stability poor, sensitivity of prepared modified electrode and it is selectively low the problems such as.As carbon materials
Expect the newcomer of family, graphene possesses the specific surface area bigger than carbon nanotube, more excellent electric conductivity and mechanical strength,
Host material as modified electrode has bigger researching value and application prospect.CoFe2O4It is a kind of important spinel-type
Magnetic material, due to having higher coercivity, preferable saturation magnetization, preferable stability and higher hardness by
It is widely used in the exploitation of new function material.
Summary of the invention
In order to overcome nanocomposite in the prior art to be used to prepare paracetamol chemical electrode, there are electrodes to stablize
Property poor, sensitivity and selectivity it is low the problems such as, primary technical problem to be solved by this invention is to provide a kind of CoFe2O4NWs/
RGO nanocomposite.
Another technical problem to be solved by this invention is to provide a kind of above-mentioned CoFe of utilization2O4NWs/RGO is nano combined
The paracetamol chemical electrode or paracetamol electrochemical sensor that material is prepared.
Above-mentioned technical problem to be solved by this invention, is achieved by the following technical programs:
A kind of CoFe2O4The preparation method of NWs/RGO nanocomposite, comprises the following steps:
S11. graphene oxide (GO) is first placed in water 10~30min of ultrasound, citric acid is then added and continues ultrasound 10
~60min obtains graphene oxide (GO) dispersion liquid；
S12. by FeCl3·6H2O and CoCl2·6H2O is added in graphene oxide (GO) dispersion liquid, ultrasonic treatment 10
~60min；
S13. pH value is adjusted to 9.5~10.5, and hydrazine is added, stirs 30~120min, is aged 18~48h；
S14. it is centrifuged, washs, obtains CoFe after drying2O4NWs/RGO nanocomposite.
Above-mentioned CoFe2O4NWs in NWs/RGO represents nano wire, is the contracting of the English name nano wires of nano wire
It writes；RGO represents redox graphene.
Preferably, the amount ratio of the graphene oxide in step S11, water and citric acid be 20~30mg:20~
30mL:2~3g.
Most preferably, the amount ratio of the graphene oxide in step S11, water and citric acid is 25mg:25mL:2.5g.
Preferably, FeCl in step S123·6H2O、CoCl2·6H2The amount ratio of O and graphene oxide (GO) dispersion liquid
For 0.4~0.5g:0.1~0.3g:20~40mL.
Most preferably, FeCl in step S123·6H2O、CoCl2·6H2The dosage of O and graphene oxide (GO) dispersion liquid
Than for 0.46g:0.2g:25mL.
Preferably, in step S13 the amount ratio of the additional amount of hydrazine and graphene oxide (GO) dispersion liquid be 1.0g:20~
40mL。
Most preferably, the amount ratio of the additional amount of hydrazine and graphene oxide (GO) dispersion liquid is 1.0g in step S13:
25mL。
Preferably, graphene oxide (GO) is first placed in water 20~30min of ultrasound in step S11, lemon is then added
Acid continues 30~40min of ultrasound, and the water is distilled water；20~30min is ultrasonically treated in step S12.
Preferably, pH value is adjusted in step S13 to 10, hydrazine is added, and stirs 40~60min, ageing 20~for 24 hours.
For using nanocomposite preparation to measure the electrode of certain specific chemical composition content, then inventor's root is needed
Different nanocomposites is prepared according to the property of specific chemical substance to be determined.The electrode prepared is to the substance of being measured
The quality of detection limit, sensitivity, stability and anti-interference and other effects mainly determined by the preparation method of nanocomposite.
The preparation method of nanocomposite mainly includes the proportion and each step reaction condition of the selection of raw material, raw material
Deng.For being used as the nanocomposite of electrode, selection, proportion and each step reaction item of preparation method chinese raw materials
The difference of part can all lead to the greatest differences of the subsequent electrode electrical property being prepared, so as to cause detection limit, sensitivity, stabilization
The greatest differences of property and anti-interference and other effects.
Inventor studies through a large number of experiments, and nano wire is prepared under above-mentioned condition parameter in invention for the first time
The CoFe of shape2O4NWs/RGO nanocomposite, the nano wire its thickness more uniformly, without obvious agglomeration, nanometer
Linear diameter is between 50-100nm.Work as CoFe2O4The nanowire supported stacking that graphene sheet layer is effectively reduced on RGO is existing
As increasing the specific surface area active of nanocomposite, being effectively improved it so that netted porous structure occurs in graphene
Electro catalytic activity, be conducive to be promoted the modified electrode that nanocomposite of the present invention is prepared detection performance (such as stability,
Sensitivity, detection limit and selectivity).
A kind of preparation method of paracetamol chemical electrode, comprises the following steps:
S21. the CoFe above-mentioned preparation method being prepared2O4NWs/RGO nanocomposite is added to organic solvent
In, ultrasonic disperse obtains CoFe2O4NWs/RGO nanocomposite dispersion liquid；
S22. by the CoFe2O4NWs/RGO nanocomposite dispersant liquid drop is added to glassy carbon electrode surface, and drying is
Obtain the paracetamol chemical electrode.
Preferably, organic solvent described in step S21 is dimethylformamide (DMF), the CoFe2O4NWs/RGO
The amount ratio of nanocomposite and dimethylformamide is 3~6mg:8~12mL.
Most preferably, the CoFe2O4The amount ratio of NWs/RGO nanocomposite and dimethylformamide is 5mg:
10mL。
A kind of preparation method of paracetamol electrochemical sensor is with the above-mentioned paracetamol chemical electrode being prepared
It is that reference electrode constitutes three-electrode system that working electrode, platinum electrode, which are to electrode, saturated calomel electrode, by three-electrode system group
It is connected after dress with electrochemical workstation and constitutes electrochemical sensor.
The present invention utilizes in-situ chemical route by the CoFe of structure novel2O4It is nanowire supported at redox graphene (RGO)
On, it is based on CoFe2O4NWs/RGO nanocomposite building paracetamol electrochemical sensor not yet appears in the newspapers.
The paracetamol chemical electrode that is prepared according to the above method flutters hot breath according to what the above method was prepared
Application of the pain electrochemical sensor in measurement drug in paracetamol content.Concrete application method are as follows: flutter hot breath using above-mentioned
Pain electrochemical sensor measures the lemon of pH 8.0 using cyclic voltammetry when enrichment time is 120s, to sweep speed be 100 mV/s
The paracetamol of various concentration in lemon acid-disodium hydrogen phosphate bottom liquid, and make paracetamol concentration and its oxidation peak current value it
Between linear relationship chart, obtain linear equation；Its current-responsive is measured after commercially available paracetamol tablet is pulverized, dissolves and filtered
Value calculates the content of paracetamol in tablet according to linear equation；The linear equation are as follows: Ip(μ A)=0.0911c (10- 5mol/L)+2.305×10-7(R2=0.9918), c is paracetamol concentration, I in the equationpIt is aoxidized for cyclic voltammetry
Peak point current.
The utility model has the advantages that the CoFe of nanometer threadiness is prepared in (1) present invention for the first time2O4It is supported on RGO lamella and forms nanometer
Composite material, the nano wire its thickness more uniformly, without obvious agglomeration, the composite active specific surface area
Greatly, electro catalytic activity is good；(2) CoFe is utilized2O4The chemical electrode or electricity that NWs/RGO nanocomposite is prepared
Chemical sensor have during measuring paracetamol stability is good, detection limit it is low (embodiment show its detection be limited to 3.9 ×
10-9Mol/L), sensitivity and selective high advantage；(3) electrochemical sensor described in is able to achieve paracetamol in drug
Field quick detection, have many advantages, such as it is easy to carry, easy to operate, low in cost, drug safety, in terms of have
Broad application prospect.
Detailed description of the invention
Fig. 1 is RGO (A) and CoFe of the present invention2O4The scanning electron microscope (SEM) photograph of NWs/RGO nanocomposite (B).
Fig. 2 is CoFe of the present invention2O4The energy spectrum diagram of NWs/RGO nanocomposite.
Fig. 3 is GCE (a), RGO/GCE (b) and paracetamol chemical electrode (c) of the present invention in 5.0mmol/L
K3[Fe(CN)6] and AC impedance (A) and cyclic voltammogram (B) in the liquid of the bottom 10mmol/L KCl.
Fig. 4 is that GCE (a), RGO/GCE (b) and paracetamol chemical electrode (c) of the present invention are flutterred in 1.0mmol/L
Cyclic voltammogram in heat breath pain solution.
Fig. 5 is cyclic voltammetry curve of the various concentration paracetamol on paracetamol chemical electrode of the present invention
(A), the linear relationship chart (B) between paracetamol concentration and its oxidation peak current value.
Specific embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of limit to the present invention
It is fixed.
Embodiment 1CoFe2O4The preparation of NWs/RGO nanocomposite
S11. graphene oxide (GO) is first placed in water ultrasonic 20min, citric acid is then added and continues ultrasound 30min,
Obtain graphene oxide (GO) dispersion liquid；
S12. by FeCl3·6H2O and CoCl2·6H2O is added in graphene oxide (GO) dispersion liquid, ultrasonic treatment
20min；
S13. pH value is adjusted to 9.5~10.5, and hydrazine is added, stirs 60min, ageing is for 24 hours；
S14. it is centrifuged, washs, obtains CoFe after drying2O4NWs/RGO nanocomposite；
The amount ratio of graphene oxide, water and citric acid in step S11 is 25mg:25mL:2.5g；
FeCl in step S123·6H2O、CoCl2·6H2The amount ratio of O and graphene oxide (GO) dispersion liquid is 0.46g:
0.2g:25mL；
The amount ratio of the additional amount of hydrazine and graphene oxide (GO) dispersion liquid is 1.0g:25mL in step S13.
Visible RGO lamella has typical pleated structure from Figure 1A, but due to π-π effect and intermolecular Van der Waals
Power, there is also stacking phenomenons between lamella.As it can be seen that CoFe from Figure 1B2O4Nano wire successfully synthesizes, thickness more uniformly,
Without obvious agglomeration, nanowire diameter is between 50-100nm.Work as CoFe2O4It is nanowire supported also to be effectively reduced on RGO
The stacking phenomenon of graphene sheet layer, so that netted porous structure occurs in graphene, the activity for increasing composite membrane compares table
Area is effectively improved its electro catalytic activity, is conducive to the detection performance for enhancing complex film modified electrode.
It can be seen in fig. 2 that mainly containing the elements such as C, O, Co, Fe in composite material, it was confirmed that Co, Fe element in the present invention
It is successfully supported on graphene-based bottom.The atomic ratio of Co and Fe element is also close to 1:2, mole of this and ferrite chemical formula simultaneously
Than being consistent, illustrate that iron cobalt salt prepared by the present invention is CoFe2O4.In addition, Si, Au element occurred in Fig. 2 is sample test
Introduce in the process, mainly sample test when sample substrate and gold-plated caused.
The preparation of 2 paracetamol chemical electrode of embodiment
S21. CoFe embodiment 1 being prepared2O4NWs/RGO nanocomposite is added in organic solvent, ultrasound
Dispersion, obtains CoFe2O4NWs/RGO nanocomposite dispersion liquid；
S22. by the CoFe2O4NWs/RGO nanocomposite dispersant liquid drop is added to glassy carbon electrode surface, and drying is
Obtain the paracetamol chemical electrode；
Organic solvent described in step S21 is dimethylformamide (DMF), the CoFe2O4NWs/RGO is nano combined
The amount ratio of material and dimethylformamide is 5mg:10mL.
A kind of preparation of the paracetamol electrochemical sensor of embodiment 3
The paracetamol chemical electrode being prepared using embodiment 2 is sweet to electrode, saturation as working electrode, platinum electrode
Mercury electrode is that reference electrode constitutes three-electrode system, is connected after three-electrode system is assembled with electrochemical workstation and constitutes electrochemistry
Sensor.
The performance test of 4 paracetamol chemical electrode of embodiment
The paracetamol chemical electrode being prepared using embodiment 2 tests its following performance as test object:
(1) electrochemical property test
In the three electrode test systems that such as embodiment 3 is prepared, respectively with GCE (a), RGO/GCE (b) and implementation
The paracetamol chemical electrode (c) that example 2 is prepared is working electrode in 5.0mmol/L K3[Fe(CN)6] it is mixed with 10mmol/
AC impedance (A) and cyclic voltammogram (B) test, test condition are as follows: frequency range 10 are carried out in the bottom liquid of L KCl5~
0.1HZ, amplitude 5mV, current potential 0.17V, test result such as Fig. 3.Half circular diameter of AC impedance figure represents electrode surface electronics and turns
Move impedance (Ret) relative size.As can be seen from Figure 3A, the R of probe ionetImpedance is in CoFe2O4NWs/RGO is nano combined
Minimum (about 800 Ω) on material, illustrates that the electron transfer capacity of paracetamol chemical electrode of the present invention is much better than list
The RGO electrode and bare electrode of component.As it can be seen that comparing GCE and RGO/GCE from Fig. 3 B, probe ion is flutterred of the present invention
Redox peak current on heat breath pain chemical electrode is maximum (120 μ A)；Illustrate the CoFe that the present invention is prepared2O4NWs/
The catalytic performance and accumulation ability of RGO nanocomposite are stronger, so as to improve the electrochemical response ability of modified electrode, have
Conducive to the sensitivity and detection limit for promoting sensor.
(2) electrocatalysis characteristic is tested
Fig. 4 is that GCE (a), RGO/GCE (b) and paracetamol chemical electrode (c) of the present invention are flutterred in 1.0mmol/L
Cyclic voltammogram in heat breath pain solution.Cyclic voltammetry experiment condition are as follows: enrichment time 120s, to sweep speed be 100mV/s, from
There is apparent redox peaks, spike potential on paracetamol chemical electrode of the present invention in visible paracetamol in Fig. 4
Respectively 0.430V and 0.001V, and its oxidation peak current (125 μ A) is maximum on three electrodes, illustrates that the present invention is prepared
CoFe2O4NWs/RGO nanocomposite has preferable electrocatalytic oxidation to act on paracetamol, is conducive to promote the biography
Detection performance of the sensor to paracetamol.
(3) detection limit is tested
The citrate-phosphate of pH 8.0 is measured when enrichment time is 120s, to sweep speed be 100mV/s using cyclic voltammetry
The paracetamol of various concentration in the liquid of disodium hydrogen bottom, and make the linear pass between paracetamol concentration and its oxidation peak current value
System's figure, obtains linear equation；From Fig. 5 A as it can be seen that the oxidation peak current value of paracetamol increases with the increase of its concentration, and
In oxidation peak current and its concentration 8 × 10-7~1 × 10-5It is in a linear relationship in the range of mol/L.Fig. 5 B gives linear side
Journey are as follows: Ip(μ A)=0.0911c (10-5mol/L)+ 2.305×10-7(R2=0.9918), c is that paracetamol is dense in the equation
Degree, IpOxidation peak current value is obtained for cyclic voltammetry；3.9 × 10 are limited to according to the detection of three times signal-to-noise ratio computation-9mol/L。
(4) stability test
8 paracetamol chemical electrodes are prepared under 2 the same terms of embodiment under same experiment condition to 1.0 × 10- 3The paracetamol of mol/L is measured respectively, and the relative standard deviation (RSD) of measurement result is 3.41%；And in 8 differences
Period (testing 1 time for the 1st day, be spaced 1 day and test 1 time) is measured with same branch paracetamol chemical electrode, show that RSD is
3.68%.In the range of relative standard deviation allows, it is preferable that this illustrates that paracetamol chemical electrode of the present invention has
Stability and reproducibility, can be used for the detection of paracetamol content in actual sample.
(5) anti-interference capability testing
Using cyclic voltammetry investigated levodopa amine, urea, ascorbic acid, adenine VB1, caffeic acid, 1- naphthols,
The influence that bisphenol-A measures paracetamol.Firstly, taking 8 0.5mL paracetamol (1.0 × 10 is housed-3) and 4.5mL lemon mol/L
Lemon acid-disodium hydrogen phosphate (pH=8.0) is the reagent bottle of bottom liquid, (enrichment time 120s, is swept speed with cyclic voltammetry and is
It is measured respectively 100mV/s), and sequentially adds above 1.0 × 10 into this 8 reagent bottles again respectively-3Mol/L's is dry
Substance 0.5mL is disturbed, is measured using identical method.As it can be seen from table 1 the variation of these oxidation peak current values is less,
(detected value deviation is ± 5%) above interfering substance is on the measurement of paracetamol substantially without influence, table in allowable range of error
Bright paracetamol chemical electrode prepared by the present invention has preferable anti-interference ability.
The influence that 1 chaff interferent of table measures paracetamol
The detection of 5 actual sample of embodiment
Actual sample is by the paracetamol tablets of the europeanized Co., Ltd's production in Guangzhou, and major auxiliary burden is microcrystalline cellulose
Element, hydroxypropylcellulose, magnesium stearate, silicon dichloride, sodium carboxymethylstarch, hydroxypropyl methylcellulose, dodecyl sodium sulfate, poly- second two
Alcohol -6000, titanium chloride, talcum powder etc., the tablet attending effectiveness are used for fever caused by common cold or influenza,
It such as has a headache for alleviating mild to moderate pain, arthralgia, migraine, toothache, courbature neuralgia.Firstly, take 1 to second
Acylamino phenol piece (weight 0.5g), is ground, weighs 0.15g therein and be dissolved in 50mL dehydrated alcohol, sonic oscillation
30min is completely dissolved in the paracetamol wherein contained in dehydrated alcohol, then stands filtering, removes filter residue, sample needed for being made
Product liquid.The above-mentioned sample liquid that 2mL is added in the bottom citrate-phosphate disodium hydrogen (pH=8.0) liquid of 5mL carries out cyclic voltammetry
Measurement result is substituted into linear equation (linear equation are as follows: I by (enrichment time 120s, sweep speed be 100mV/s) measurementp(μ A)=
0.0911c(10-5mol/L)+2.305×10-7(R2=0.9918), c is paracetamol concentration, I in the equationpFor circulation volt
Peace method obtains oxidation peak current value) in be computed in every tablet of tablet containing paracetamol 0.258g.Then toward according to the method described above
The standard solution of 2mL, 4mL, 6mL, 8mL, 10mL are separately added into 6 bottles of prepare liquids being made into, using cyclic voltammetry to sample
Paracetamol content in liquid is further detected, and the rate of recovery of measurement result is between 99.2%~100.3%.
Claims (4)
1. a kind of application of paracetamol electrochemical sensor in measurement drug in paracetamol content；Concrete application method
Are as follows: paracetamol electrochemical sensor is used, cyclic voltammetry survey when enrichment time is 120s, to sweep speed be 100mV/s is utilized
Determine the paracetamol of various concentration in the citrate-phosphate disodium hydrogen bottom liquid of pH 8.0, and makes paracetamol concentration and its oxygen
Change the linear relationship chart between peak point current, obtains linear equation；It is surveyed after commercially available paracetamol tablet is pulverized, dissolves and filtered
Its fixed current-responsive value calculates the content of paracetamol in tablet according to linear equation；The linear equation are as follows: Ip=
0.0911c+2.305×10-7, R2=0.9918；C is paracetamol concentration, unit 10 in the equation-5mol/L；Ip is circulation
Voltammetry obtains oxidation peak current value, and unit is μ A；
The paracetamol electrochemical sensor is to electrode, full by working electrode, platinum electrode of paracetamol chemical electrode
It is that reference electrode constitutes three-electrode system with calomel electrode, be connected after three-electrode system is assembled with electrochemical workstation composition electricity
Chemical sensor；
The preparation method of the paracetamol chemical electrode, it includes following steps:
S21. by CoFe2O4NWs/RGO nanocomposite is added in organic solvent, and ultrasonic disperse obtains CoFe2O4NWs/RGO
Nanocomposite dispersion liquid；
S22. by the CoFe2O4NWs/RGO nanocomposite dispersant liquid drop is added to glassy carbon electrode surface, is drying to obtain institute
The paracetamol chemical electrode stated；
The CoFe2O4NWs/RGO nanocomposite is prepared by the inclusion of the method for following steps:
S11., graphene oxide is first placed in water to 10~30min of ultrasound, citric acid is then added and continues 10~60min of ultrasound,
Obtain graphene oxide dispersion；
S12. by FeCl3·6H2O and CoCl2·6H2O is added in graphene oxide dispersion, is ultrasonically treated 10~60min；
S13. pH value is adjusted to 9.5~10.5, and hydrazine is added, stirs 30~120min, is aged 18~48h；
S14. it is centrifuged, washs, obtains CoFe after drying2O4NWs/RGO nanocomposite；
The amount ratio of graphene oxide, water and citric acid in step S11 is 25mg:25mL:2.5g；
FeCl in step S123·6H2O、CoCl2·6H2O and the amount ratio of graphene oxide dispersion are 0.46g:0.2g:
25mL；
The amount ratio of the additional amount and graphene oxide dispersion of hydrazine is 1.0g:25mL in step S13；
Organic solvent described in step S21 is dimethylformamide, the CoFe2O4NWs/RGO nanocomposite and diformazan
The amount ratio of base formamide is 3~6mg:8~12mL.
2. application according to claim 1, which is characterized in that graphene oxide is first placed in water ultrasound in step S11
Then 20~30min is added citric acid and continues 30~40min of ultrasound, the water is distilled water；It is ultrasonically treated in step S12
20~30min.
3. application according to claim 1, which is characterized in that adjust pH value in step S13 to 10, hydrazine, stirring 40 is added
~60min, ageing 20~for 24 hours.
4. application according to claim 1, which is characterized in that the CoFe2O4NWs/RGO nanocomposite and diformazan
The amount ratio of base formamide is 5mg:10mL.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610542075.1A CN106248766B (en) | 2016-07-11 | 2016-07-11 | A kind of application of electrochemical sensor in measurement drug in paracetamol content |
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| CN201610542075.1A CN106248766B (en) | 2016-07-11 | 2016-07-11 | A kind of application of electrochemical sensor in measurement drug in paracetamol content |
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| Publication Number | Publication Date |
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| CN106248766A CN106248766A (en) | 2016-12-21 |
| CN106248766B true CN106248766B (en) | 2019-07-26 |
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| CN107843627A (en) * | 2017-10-30 | 2018-03-27 | 上海应用技术大学 | Electrochemical sensor for practolol detection and preparation method thereof |
| CN108333242A (en) * | 2017-12-31 | 2018-07-27 | 苏州南尔材料科技有限公司 | A kind of preparation method of nano-cellulose cobalt acid nickel sensor material |
| CN109164083B (en) | 2018-11-13 | 2019-06-14 | 青岛大学 | Based on copper nano-cluster/carbon dots/arginine complex paracetamol ratio fluorescent sensor preparation method |
| CN111272843B (en) * | 2020-02-25 | 2023-01-06 | 衡阳师范学院 | Nano material with FeCo network structure constructed by nano wires and preparation method and application thereof |
| CN111793393B (en) * | 2020-06-29 | 2022-03-08 | 重庆第二师范学院 | Nanocomposite material, glassy carbon composite electrode, manufacturing methods of nanocomposite material and glassy carbon composite electrode, and electrochemical sensor |
| CN112611792B (en) * | 2020-12-01 | 2022-09-27 | 常州大学 | Multi-walled carbon nanotube/cobaltosic oxide for preparing electrochemical sensor for detecting caffeic acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866188A (en) * | 2012-10-27 | 2013-01-09 | 信阳师范学院 | Molybdenum sulfide-graphene electrochemical sensor and preparation method and application thereof |
| CN103018304A (en) * | 2013-01-08 | 2013-04-03 | 上海师范大学 | Glassy carbon electrode modified by nickel oxide-graphene nano material, preparation method and application thereof |
| CN103604858A (en) * | 2013-11-20 | 2014-02-26 | 南京理工大学 | Electrochemical detection method of acetaminophen medicine by PEDOT (Polymer Ethylenedioxy Thiophene)/GO (Graphene Oxide)/GCE (Glassy Carbon Electrode) |
| CN104359956A (en) * | 2014-11-19 | 2015-02-18 | 西北师范大学 | Modified electrode for detecting acetamidophenol as well as preparation and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103399063B (en) * | 2013-08-07 | 2015-07-08 | 上海师范大学 | Graphene nano material-modified glassy carbon electrode based on phytic acid dispersion, preparation method and application |
| CN105572189A (en) * | 2014-10-17 | 2016-05-11 | 南京理工大学 | Polyglutamic acid modified electrode and application thereof to detection of content of drug paracetamol |
-
2016
- 2016-07-11 CN CN201610542075.1A patent/CN106248766B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866188A (en) * | 2012-10-27 | 2013-01-09 | 信阳师范学院 | Molybdenum sulfide-graphene electrochemical sensor and preparation method and application thereof |
| CN103018304A (en) * | 2013-01-08 | 2013-04-03 | 上海师范大学 | Glassy carbon electrode modified by nickel oxide-graphene nano material, preparation method and application thereof |
| CN103604858A (en) * | 2013-11-20 | 2014-02-26 | 南京理工大学 | Electrochemical detection method of acetaminophen medicine by PEDOT (Polymer Ethylenedioxy Thiophene)/GO (Graphene Oxide)/GCE (Glassy Carbon Electrode) |
| CN104359956A (en) * | 2014-11-19 | 2015-02-18 | 西北师范大学 | Modified electrode for detecting acetamidophenol as well as preparation and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《Fabrication of cobalt ferrite nanostructures and comparison of their electrochemical properties》;D.H.Deng 等;《Cryst.Res.Technol.》;20120709;1-7页 |
| 《MnFe2O4@CNT-N as novel electrochemical nanosensor for determination of caffeine, acetaminophen and ascorbic acid》;Diana M.Fernandes 等;《Sensors and Actuators B: Chemical》;20150512;128-136页 |
| 《One-pot in situ synthesis of a CoFe2O4 nanoparticle-reduced graphene oxide nanocomposite with high performance for levodopa sensing》;Junhua Li 等;《RSC Advances》;20151116(第5期);99669-99677页 |
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