CN107315041A - Nano cupric oxide modified electrode and the method that nifedipine is analyzed with modified electrode - Google Patents
Nano cupric oxide modified electrode and the method that nifedipine is analyzed with modified electrode Download PDFInfo
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- CN107315041A CN107315041A CN201710778035.1A CN201710778035A CN107315041A CN 107315041 A CN107315041 A CN 107315041A CN 201710778035 A CN201710778035 A CN 201710778035A CN 107315041 A CN107315041 A CN 107315041A
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Abstract
The invention discloses a kind of nano cupric oxide modified electrode method, including prepare the steps such as nano cupric oxide, preparation of nano cupric oxide suspension and modified glassy carbon electrode.Invention additionally discloses a kind of method that nifedipine is analyzed with modified electrode, including step：Prepare nifedipine mother liquor；Prepare buffer solution；Foregoing nano cupric oxide modified electrode is provided；Nifedipine solution is added in buffer solution, by the use of the nano cupric oxide modified electrode in above-mentioned steps as working electrode, platinum electrode is used as corresponding reference electrode as auxiliary electrode, calomel electrode, three-electrode system is collectively constituted, nifedipine content is detected with cyclic voltammetry.The present invention obtains nano cupric oxide modified electrode by the method for nano cupric oxide modified glassy carbon electrode, and analyzes nifedipine with modified electrode, and good reproducibility of analysis results, stability are high.
Description
Technical field
The present invention relates to field of nanometer material technology, the method and modified electrode of especially a kind of nano cupric oxide modified electrode
Application in nifedipine analysis.
Background technology
Nifedipine is a class calcium antagonist, can effectively treat hypertension, prevent anginal benign pharmaceutical, be 20
The century 70 mid-term medicine obtains good reputation all over the world.It can mainly be expressed as：Curative effect is especially fast, can cause
Neurohumoral activation, by studying for many years and application practice, the medicine has obtained the accreditation of vast medical patient in the world of medicine.
The method that predominantly detects for nifedipine is divided into high performance liquid chromatography, ultraviolet spectrophotometry, voltammetry, nuclear magnetic resonance at present
Method.These methods can not fully meet requirement in terms of reappearance, stability, cost, it is therefore desirable to a kind of new analysis
Method analyzes detection nifedipine.
The content of the invention
The present invention provides a kind of high nano cupric oxide modified electrode method of favorable reproducibility, stability and uses modified electrode
The method for analyzing nifedipine.
To achieve the above object, technical scheme is as follows：
A kind of nano cupric oxide modified electrode method, comprises the following steps：
S10, prepares nano cupric oxide：Polyethylene glycol is added in acetic acid copper solution, solution A is formed；In sodium carbonate liquor
Middle addition polyethylene glycol, forms B solution after dissolving, be then uniformly added drop-wise to solution B in solution A under conditions of ultrasound, then
Ultrasonic appropriate time, finally magnetic agitation obtains black precipitate after 30 minutes under conditions of 78 DEG C, is centrifuged, instead
Multiple repeatedly washing, vacuum drying obtains copper oxide nano material；
S20, preparation of nano cupric oxide suspension：Cupric oxide nano powder is weighed, is placed in sample cell, then is added dropwise thereto
Distilled water, the mass ratio for making cupric oxide nano powder and water is 1:200, stir 5-10 minutes, then added into suspension
1.00mL1%PVP, is finally placed in the scattered 30min of concussion in ultrasonic cleaner standby by sample cell；Before each is used again
Secondary concussion 15-20min, so that nano cupric oxide particle can be uniformly dispersed；
S30, modified glassy carbon electrode：First glass-carbon electrode is placed on alundum (Al2O3) powder and carries out polishing grinding, then will
Glass-carbon electrode is placed in concussion cleaning 5-10min in the beaker for fill dilute sulfuric acid, then takes out and is cleaned with distilled water, is finally placed in room
Temperature is lower to be air-dried；Above-mentioned just finely dispersed 10 microlitres of cupric oxide nano suspension is drawn with micro syringe, is dripped using drop-coating
The electrode wicking surface of glass-carbon electrode is coated in, is subsequently placed under infrared light and dries, obtain surface nano oxidized full of very thin one layer
The modified electrode of copper particle.
A kind of method that nifedipine is analyzed with modified electrode, comprises the following steps：
S40, prepares nifedipine mother liquor；
S50, prepares buffer solution；
There is provided nano cupric oxide modified electrode as described above by S60；
S70, nifedipine solution is added in buffer solution, is made using the nano cupric oxide modified electrode in step S60
For working electrode, platinum electrode collectively constitutes three-electrode system as auxiliary electrode, calomel electrode as corresponding reference electrode,
Nifedipine content is detected with cyclic voltammetry.
In wherein step S50, buffer solution is phosphate buffer.
In wherein step S50, the pH of phosphate buffer is pH=6.80.
In wherein step S70, nano cupric oxide modified glassy carbon electrode sweep speed is 0.10V/s.
Wherein step S40 specifically includes following steps：
S41, nifedipine sample treatment：The accurate nifedipine tablets for weighing certain mass, are smashed to pieces with mortar, ground to form
Powdery granule, then adds the absolute ethyl alcohol dissolution filter of certain volume, removes insoluble matter, forms the nitre benzene of transparent clarification
Horizon sample solution, it is In Shade, need to pipette according to concentration stand-by；
S42, prepares nifedipine mother liquor：Nifedipine active compound is weighed to be placed in beaker, plus ethanol dissolving, formation 0.2 ×
10-2Mol/L nifedipine mother liquor, it is In Shade standby.
The present invention obtains nano cupric oxide modified electrode by the method for nano cupric oxide modified glassy carbon electrode, and with modifying
Electrode analysis nifedipine, good reproducibility of analysis results, stability are high.
Brief description of the drawings
Fig. 1 is CV of the nifedipine in bare glassy carbon electrode and nano cupric oxide modified glassy carbon electrode in the embodiment of the present invention
Curve map.
Fig. 2 is electrochemical response behavior comparison chart of the nifedipine in different buffer solutions in the embodiment of the present invention.
Fig. 3 is the graph of a relation of reduction current and pH in the embodiment of the present invention.
Fig. 4 is reduction current and the graph of a relation of sweep speed in the embodiment of the present invention.
Fig. 5 schemes for the DPV of the nifedipine of various concentrations under optimum condition in the embodiment of the present invention.
Fig. 6 is reduction current and the graph of a relation of nifedipine concentration in the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and example, the present invention will be further described.
In the present embodiment, nano cupric oxide modified electrode method is hanged including preparing nano cupric oxide, preparation of nano cupric oxide
Turbid three steps of liquid and modified glassy carbon electrode.
The method for preparing nano cupric oxide is：Added in acetic acid copper solution into PEG (polyethylene glycol), form solution A；
PEG (polyethylene glycol) is added in sodium carbonate liquor, B solution is formed after dissolving.Then solution B is uniformly dripped under conditions of ultrasound
It is added in solution A, then ultrasonic appropriate time, finally magnetic agitation obtains black precipitate after 30 minutes under conditions of 78 DEG C,
Centrifuged, repeated multiple times washing, vacuum drying obtains copper oxide nano material of the particle diameter for 50-70nm or so.Fig. 1
For the electron lens scanning result of the present embodiment nano cupric oxide finished product.
The preparation of nano cupric oxide suspension：0.0100g cupric oxide nano powder accurately is weighed, is placed in sample cell, then
2.00mL distilled water is added dropwise thereto, somewhat stirs 5-10 minutes, 1.00mL1%PVP (polyethylene is then added into suspension
Pyrrolidones), sample cell is finally placed in the scattered 30min of concussion in ultrasonic cleaner standby.Before each is used will
15-20min is shaken again, so that nano cupric oxide particle can be uniformly dispersed.
To the method for modifying of glass-carbon electrode：First glass-carbon electrode is placed on alundum (Al2O3) powder and carries out polishing grinding, so
Glass-carbon electrode is placed in concussion cleaning 5-10min in the beaker for fill dilute sulfuric acid afterwards, then takes out and is cleaned with distilled water, it is most rearmounted
Air-dry at room temperature.Above-mentioned just finely dispersed 10.00 microlitres of cupric oxide nano suspension is drawn with micro syringe, using drop
Coating drop coating is subsequently placed under infrared light and dried, obtain surface and received full of very thin one layer in the electrode wicking surface of glass-carbon electrode
The modified electrode of rice copper oxide particle.
In the present embodiment, comprised the following steps with modified electrode analysis nifedipine.
S40, prepares nifedipine mother liquor
Including S41, nifedipine sample treatment：The accurate nifedipine tablets for weighing certain mass, are smash with mortar
Broken, be ground into powder particle, then adds the absolute ethyl alcohol dissolution filter of certain volume, removes insoluble matter.Formed transparent
The nifedipine sample solution of clarification, it is In Shade, need to pipette according to concentration stand-by.
S42, prepares nifedipine mother liquor：Accurately 0.0693g nifedipine active compounds are weighed to be placed in beaker, plus ethanol is molten
Solution, is then settled in 100.00mL volumetric flasks, forms 0.2 × 10-2Mol/L nifedipine mother liquor, it is In Shade standby.
S50, prepares buffer solution
Influence for research different buffering bottoms liquid to nifedipine electrochemical response, the present embodiment have chosen phosphoric acid buffer
Liquid, BR buffer solutions, sodium tetraborate buffer solution, NH3-NH4Cl buffer solutions and Na2CO3-NaHCO3Buffer solution.
The principle of the present embodiment is：It regard the glass-carbon electrode modified before with nano cupric oxide as working electrode, platinum electricity
Pole collectively constitutes three-electrode system as auxiliary (to) electrode, 222 type calomel electrodes as corresponding reference electrode.With following
Ring voltammetry (CV) qualitative response for finding various medicines under the liquid of various buffering bottoms, it is then determined that optimized buffer liquid and Optimal pH
Value and sweep speed, standard curve, reappearance, minimum detectability and mark-on are quantitatively done after all determining by DPV again
Recovering state, so that deducing medicine corresponding electrochemical behavior occurs.Experimental data is recorded and preserved with electrochemical workstation.
The contrast of bare electrode and modified electrode
In Fig. 1, A is response peak current of the modified electrode to nifedipine；B is response of the bare glassy carbon electrode to nifedipine
Peak current；C is response curve of the modified electrode to phosphate buffer.Phosphate is in the interval interior nothing of response as can be drawn from Figure 1
Interference, its response is due to the electrochemical behavior of nifedipine.Curve A and B contrast find out that the electrode of cupric oxide modification is than naked electricity
The response of pole is strong, illustrates that nano-modified dose of cupric oxide serves the effect of catalytic reaction in the electrochemical behavior of nifedipine.
The selection of buffer solution
The nifedipine solution of same concentrations, same volume is added in different cushioning liquid, then with cyclic voltammetric
Method determines electrochemical behavior of the Nanoparticle Modified Electrode in different buffer solutions for nifedipine medicine.Buffer solution has respectively：Phosphorus
Acid buffer, BR buffer solutions, sodium tetraborate buffer solution, NH3-NH4Cl buffer solutions and Na2CO3-NaHCO3Buffer solution.Can from Fig. 2
To find out that the response effect of phosphate buffer (A curves) is more obvious, peak type is optimal, so determining that phosphate buffer is nitre benzene
The optimized buffer bottom liquid of ordinary telegram Chemical response.
The determination of Optimal pH
Prepare five groups of solution：Concentration is identical, phosphate-buffered bottom liquid PH be respectively 6.48,6.80,7.59,8.02 and
8.52, five group testing liquids of the composition with PH gradients.Then with three electricity of the cupric oxide nano modified electrode as working electrode
Electrode systems are detected, obtain a series of different curve of peak values.When obvious must can find out as pH=6.80 from Fig. 3, electrification
Response is learned most obvious, peak value is optimal, so determining that pH=6.80 is Optimal pH.
The determination of optimum scanning speed
A phosphate bottom liquid using PH=6.80 is prepared as the nifedipine standard liquid of buffer solution, is received in cupric oxide
Rice modified electrode for working electrode three-electrode system under detected, take sweep speed be 0.06,0.08,0.10,0.12,
0.14V/s, is repeatedly determined respectively.When can significantly finding out sweep speed from Fig. 4 for 0.1V/s, nifedipine
Electrochemical response is most strong.To sum up, nifedipine optimum response sweep speed is 0.10V/s.
The range of linearity and detection limit of nifedipine
Under optimum experimental condition, i.e. pH=6.8, under conditions of sweep speed=0.10V/s, with DPV method pair
Concentration is respectively:A in Fig. 5：1.0×10-4mol/L、B：2.0×10-4mol/L、C：3.0×10-4Mol/L has concentration gradient
Nifedipine solution tested and analyzed.The linearity curve of concentration and reduction current is produced according to Fig. 6, it can be seen from Fig. 6
Its concentration is 1.0 × 10-4Mol/L~5.0 × 10-4Linear relationship is respectively provided between mol/L scopes, its linear side is calculated
Journey is y=0.0036x+E-06, and dependent linearity coefficient is 0.9918.According to detection limit formula LOD=3 σ/(σ represents blank mark to S
Quasi- deviation, S represents calibration curve slope), its detection limit=0.7 × 10 can be calculated-8mol/L。
Reappearance, the stability of Nanoparticle Modified Electrode
Stability：Modified electrode is placed in one week at room temperature, the detection of same amount material is then carried out to nifedipine,
As a result fallen 0.12% on a year-on-year basis, illustrated having good stability for modified electrode.
Reappearance：It is 2.0 × 10 that modified electrode is repeated 10 times into measure concentration-4Mol/L nifedipine solution [16], from
From the point of view of the result of 10 measure, the relative deviation of peak current maintains 2.9%-7.1% or so, should be test result indicates that modification electricity
The reappearance of pole is relatively preferable.
The interference experiment of Nanoparticle Modified Electrode
Influence of the auxiliary material to electrochemical response of nifedipine has been investigated, has as a result been shown, more than 10 times of dextrin, sweet dew
Alcohol, calcium carbonate, methylcellulose etc. do not produce interference to experimental result.Because being frequently added thiazine hypotensor in nifedipine
Thing, excluding modified electrode parathiazine class medicine by many experiments has response；Contained antioxidant material in same medicament,
Organic solvent etc. influences also very little to its annoyance level, as a result shows that the anti-interference of cupric oxide nano modified electrode is very strong.
The calculating of nifedipine assay and recovery of standard addition
Nifedipine mark-on reclaims amount：The constant nifedipine sample solution of concentration, takes three parts of same volume respectively, plus
Enter 5.00mL phosphate buffers and carry out analysis detection at optimum conditions；Then the nifedipine of same volume determination amount is added
Carry out analysis detection after standard liquid at optimum conditions again.Calculated value after last every part of nifedipine solution mark-on,
Subtract the calculated value before mark-on, as a result both difference divided by add nifedipine standard substance be exactly recovery of standard addition feelings
Condition.
Specific standards defined formula is：
With the three-electrode system for the electrochemical workstation that nano cupric oxide modified glassy carbon electrode is working electrode, DPV methods are used
Analysis is determined, 2 are the results are shown in Table, learns that the recovery of standard addition of nifedipine is 84.2% -95.7% eventually through calculating.
The rate of recovery of the nifedipine of table 2：
Claims (6)
1. a kind of nano cupric oxide modified electrode method, it is characterised in that comprise the following steps：
S10, prepares nano cupric oxide：Polyethylene glycol is added in acetic acid copper solution, solution A is formed；Add in sodium carbonate liquor
Enter and B solution is formed after polyethylene glycol, dissolving, be then uniformly added drop-wise to solution B in solution A under conditions of ultrasound, then ultrasound
Appropriate time, finally magnetic agitation obtains black precipitate after 30 minutes under conditions of 78 DEG C, is centrifuged, repeatedly many
Secondary washing, vacuum drying obtains copper oxide nano material；
S20, preparation of nano cupric oxide suspension：Cupric oxide nano powder is weighed, is placed in sample cell, then distillation is added dropwise thereto
Water, the mass ratio for making cupric oxide nano powder and water is 1:200, stir 5-10 minutes, then added into suspension
1.00mL1%PVP, is finally placed in the scattered 30min of concussion in ultrasonic cleaner standby by sample cell；Before each is used again
Secondary concussion 15-20min, so that nano cupric oxide particle can be uniformly dispersed；
S30, modified glassy carbon electrode：First glass-carbon electrode is placed on alundum (Al2O3) powder and carries out polishing grinding, then by glass carbon
Electrode is placed in concussion cleaning 5-10min in the beaker for fill dilute sulfuric acid, then takes out and is cleaned with distilled water, is finally placed at room temperature
Air-dry；Above-mentioned just finely dispersed 10 microlitres of cupric oxide nano suspension is drawn with micro syringe, is existed using drop-coating drop coating
The electrode wicking surface of glass-carbon electrode, is subsequently placed under infrared light and dries, and obtains surface full of one layer of very thin nano cupric oxide
The modified electrode of grain.
2. a kind of method that nifedipine is analyzed with modified electrode, it is characterised in that comprise the following steps：
S40, prepares nifedipine mother liquor；
S50, prepares buffer solution；
There is provided nano cupric oxide modified electrode as claimed in claim 1 by S60；
S70, nifedipine solution is added in buffer solution, and work is used as by the use of the nano cupric oxide modified electrode in step S60
Make electrode, platinum electrode is as auxiliary electrode, and calomel electrode collectively constitutes three-electrode system as corresponding reference electrode, use
Cyclic voltammetry detects nifedipine content.
3. method as claimed in claim 2, it is characterised in that in wherein step S50, buffer solution is phosphate buffer.
4. method as claimed in claim 3, it is characterised in that in wherein step S50, the pH of phosphate buffer is pH=
6.80。
5. method as claimed in claim 4, it is characterised in that in wherein step S70, nano cupric oxide modified glassy carbon electrode is swept
Speed is retouched for 0.10V/s.
6. method as claimed in claim 2, it is characterised in that wherein step S40 specifically includes following steps：
S41, nifedipine sample treatment：The nifedipine tablets of certain mass are weighed, are smashed to pieces with mortar, are ground into powder
Grain, then adds the absolute ethyl alcohol dissolution filter of certain volume, removes insoluble matter, forms the nifedipine sample of transparent clarification
Solution, it is In Shade, need to pipette according to concentration stand-by；
S42, prepares nifedipine mother liquor：Nifedipine active compound is weighed to be placed in beaker, plus ethanol dissolving, form 0.2 × 10- 2Mol/L nifedipine mother liquor, it is In Shade standby.
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| CN108459062A (en) * | 2017-09-01 | 2018-08-28 | 湖南工程学院 | Nano cupric oxide modified electrode and the method for replacing meter Sha Xing with modified electrode analysis |
| CN108459062B (en) * | 2017-09-01 | 2020-06-26 | 湖南工程学院 | Nano copper oxide modified electrode and method for analyzing tilmicosin by using modified electrode |
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