CN107315041B - Nano cupric oxide modified electrode and the method with modified electrode analysis nifedipine - Google Patents

Nano cupric oxide modified electrode and the method with modified electrode analysis nifedipine Download PDF

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CN107315041B
CN107315041B CN201710778035.1A CN201710778035A CN107315041B CN 107315041 B CN107315041 B CN 107315041B CN 201710778035 A CN201710778035 A CN 201710778035A CN 107315041 B CN107315041 B CN 107315041B
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electrode
nifedipine
cupric oxide
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CN107315041A (en
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陈立新
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Hunan Institute of Engineering
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    • G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
    • 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
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Abstract

The invention discloses a kind of nano cupric oxide modified electrode method, including preparing nano cupric oxide, preparation of nano copper oxide suspension and modified glassy carbon electrode.Invention additionally discloses a kind of method with modified electrode analysis nifedipine, including step：Prepare nifedipine mother liquor；Prepare buffer solution；Aforementioned 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 as auxiliary electrode, and calomel electrode is as corresponding reference electrode, three-electrode system is collectively constituted, nifedipine content is detected with cyclic voltammetry.The present invention obtains nano cupric oxide modified electrode, and analyze nifedipine with modified electrode by the method for nano cupric oxide modified glassy carbon electrode, and good reproducibility of analysis results, stability are high.

Description

Nano cupric oxide modified electrode and the method with modified electrode analysis nifedipine
Technical field
The present invention relates to field of nanometer material technology, the especially a kind of method and modified electrode of nano cupric oxide modified electrode Application in nifedipine analysis.
Background technology
Nifedipine is a kind of calcium antagonist, can effectively treat hypertension, the anginal benign pharmaceutical of prevention, be 20 The century 70 mid-term drug 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 drug have obtained the accreditation of vast medical patient in the world of medicine. High performance liquid chromatography, ultraviolet spectrophotometry, voltammetry, nuclear magnetic resonance are divided into for the method that predominantly detects of nifedipine at present Method.These methods cannot fully meet requirement in reproducibility, stability, cost etc., it is therefore desirable to a kind of novel analysis Method analyzes detection nifedipine.
Invention content
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, includes the following steps：
S10 prepares nano cupric oxide：Polyethylene glycol is added in acetic acid copper solution, forms solution A；In sodium carbonate liquor Middle addition polyethylene glycol, forms B solution after dissolving, during solution B then is dropped evenly 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 obtain copper oxide nano material；
S20, preparation of nano copper oxide suspension：Cupric oxide nano powder is weighed, is placed in sample cell, then is added dropwise thereto Distilled water, it is 1 to make the mass ratio of cupric oxide nano powder and water:200, it stirs 5-10 minutes, is then added in into suspension It is spare to be finally placed in concussion dispersion 30min in ultrasonic cleaner by 1.00mL1%PVP for 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, it is nano oxidized full of very thin one layer to obtain surface The modified electrode of copper particle.
A kind of method with modified electrode analysis nifedipine includes the following steps：
S40 prepares nifedipine mother liquor；
S50 prepares buffer solution；
S60 provides nano cupric oxide modified electrode as described above；
Nifedipine solution is added in buffer solution by S70, is made using the nano cupric oxide modified electrode in step S60 For working electrode, for platinum electrode as auxiliary electrode, calomel electrode collectively constitutes three-electrode system 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 comprises the following steps：
S41, nifedipine sample treatment：The accurate nifedipine tablets for weighing certain mass, are smashed to pieces with mortar, are ground into Then powdery granule adds in the absolute ethyl alcohol dissolution filter of certain volume, remove insoluble matter, forms transparent clear nitre benzene Horizon sample solution, it is In Shade, it is pipetted according to concentration needs for use；
S42 prepares nifedipine mother liquor：It weighs nifedipine active compound to be placed in beaker, ethyl alcohol is added to dissolve, formation 0.2 × 10-2The nifedipine mother liquor of mol/L, it is In Shade spare.
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.
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 graph.
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 relational graph of reduction current and pH in the embodiment of the present invention.
Fig. 4 is the relational graph of reduction current and sweep speed in the embodiment of the present invention.
Fig. 5 is the DPV figures of the nifedipine of various concentration under optimum condition in the embodiment of the present invention.
Fig. 6 is reduction current and the relational graph of nifedipine concentration in the embodiment of the present invention.
Specific 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 including preparing nano cupric oxide, preparation of nano copper oxide hangs Three steps of turbid and modified glassy carbon electrode.
The method for preparing nano cupric oxide is：It is added in acetic acid copper solution into PEG (polyethylene glycol), forms 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, It is centrifuged, repeated multiple times washing, vacuum drying obtains copper oxide nano material of the grain size for 50-70nm or so.Fig. 1 Electron lens scanning result for 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, slightly stirs 5-10 minutes, 1.00mL1%PVP (polyethylene is then added in into suspension Pyrrolidones), it is spare that sample cell is finally placed in concussion dispersion 30min in ultrasonic cleaner.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, most postposition It air-dries 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, included 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 in the absolute ethyl alcohol dissolution filter of certain volume, removes insoluble matter.It is formed transparent Clear nifedipine sample solution, it is In Shade, it is pipetted according to concentration needs for use.
S42 prepares nifedipine mother liquor：It accurately weighs 0.0693g nifedipine active compounds to be placed in beaker, adds ethyl alcohol molten Solution, is then settled in 100.00mL volumetric flasks, forms 0.2 × 10-2The nifedipine mother liquor of mol/L, it is In Shade spare.
S50 prepares buffer solution
To study influence of the different buffering bottom liquid to nifedipine electrochemical response, the present embodiment has 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：Using before by the use of the glass-carbon electrode that nano cupric oxide has been modified 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 drugs under various buffering bottom liquid, then determines optimized buffer liquid and Optimal pH Value and sweep speed quantitatively do standard curve, reproducibility, minimum detectability and mark-on by DPV again after all determining There is corresponding electrochemical behavior so as to deduce drug in recovering state.Experimental data is recorded and preserved with electrochemical workstation.
The comparison 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 nothing in response section as can be drawn from Figure 1 Interference, response are the electrochemical behaviors due to nifedipine.Curve A and B comparison find out that the electrode of copper oxide modification is than naked electricity The response of pole is strong, illustrates that nano-modified dose of copper oxide plays the role of catalysis reaction in the electrochemical behavior of nifedipine.
The selection of buffer solution
The nifedipine solution of same concentrations, same volume is added in different buffer solutions, then with cyclic voltammetric Method measures Nanoparticle Modified Electrode in different buffer solutions for the electrochemical behavior of nifedipine drug.Buffer solution has respectively：Phosphorus Acid buffer, BR buffer solutions, sodium tetraborate buffer solution, NH3-NH4Cl buffer solutions and Na2CO3-NaHCO3Buffer solution.It can from Fig. 2 To find out that the response effect of phosphate buffer (A curves) is more obvious, peak type is best, so determining phosphate buffer for nitre benzene The optimized buffer bottom liquid of ordinary telegram Chemical response.
Optimal pH determines
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 by the use of cupric oxide nano modified electrode as the three of working electrode electricity Electrode systems are detected, and obtain a series of different curve of peak values.From Fig. 3 can be apparent find out as pH=6.80 when, electrification Response is most apparent, and peak value is best, so determining that pH=6.80 is Optimal pH.
Optimum scanning rate determines
A phosphate bottom liquid using PH=6.80 is prepared as the nifedipine standard solution of buffer solution, is received in copper oxide Rice modified electrode to be detected under the three-electrode system of working electrode, take sweep speed for 0.06,0.08,0.10,0.12, 0.14V/s is repeatedly measured respectively.When can significantly finding out sweep speed for 0.1V/s from Fig. 4, 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. under conditions of pH=6.8, sweep speed=0.10V/s, with the method pair of DPV 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 be detected analysis.The linearity curve of concentration and reduction current is produced according to Fig. 6, as 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 ranges, 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/S, (σ represents blank mark Quasi- deviation, S represent calibration curve slope), its detection limit=0.7 × 10 can be calculated-8mol/L。
Reproducibility, the stability of Nanoparticle Modified Electrode
Stability：Modified electrode is placed in one week at room temperature, the detection of same amount substance is then carried out to nifedipine, As a result it has fallen 0.12% on a year-on-year basis, has illustrated having good stability for modified electrode.
Reproducibility：It is 2.0 × 10 that modified electrode is repeated 10 times measured concentration-4The nifedipine solution [16] of mol/L, 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 the experimental results showed that modification electricity The reproducibility 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, the result shows that, 10 times or more of dextrin, sweet dew Alcohol, calcium carbonate, methylcellulose etc. do not generate experimental result interference.Because thiazine hypotensor is frequently added in nifedipine Object, excluding modified electrode parathiazine class drug by many experiments has response；Contained antioxidant substance in similary medicament, Organic solvent etc. influences also very little to its annoyance level, the results showed 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, adds respectively Enter 5.00mL phosphate buffers and carry out analysis detection at optimum conditions；Then the nifedipine of the same volume amount of determining is added in Analysis detection is carried out at optimum conditions again after standard solution.Calculated value after last every part of nifedipine solution mark-on, Subtract the calculated value before mark-on, difference both as a result divided by add in 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, with DPV methods Analysis is measured, the results are shown in Table 2, learns that the recovery of standard addition of nifedipine is 84.2% -95.7% eventually by calculating.
The rate of recovery of 2 nifedipine of table：

Claims (5)

  1. A kind of 1. method with modified electrode analysis nifedipine, which is characterized in that include the following steps：
    S40 prepares nifedipine mother liquor；
    S50 prepares buffer solution；
    S60, provides nano cupric oxide modified electrode, and the nano cupric oxide modified electrode is made of following S61-S63 steps：
    S61 prepares nano cupric oxide：Polyethylene glycol is added in acetic acid copper solution, forms solution A；Add in sodium carbonate liquor Enter polyethylene glycol, B solution is formed after dissolving, during solution B then is dropped evenly 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 more Secondary washing, vacuum drying obtain copper oxide nano material；
    S62, preparation of nano copper oxide suspension：Cupric oxide nano powder is weighed, is placed in sample cell, then distillation is added dropwise thereto Water, it is 1 to make the mass ratio of cupric oxide nano powder and water:200, it stirs 5-10 minutes, is then added in into suspension It is spare to be finally placed in concussion dispersion 30min in ultrasonic cleaner by 1.00mL1%PVP for sample cell；Before each is used again Secondary concussion 15-20min, so that nano cupric oxide particle can be uniformly dispersed；
    S63, 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 It air-dries；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；
    Nifedipine solution is added in buffer solution by S70, by the use of the nano cupric oxide modified electrode in step S60 as work Make electrode, platinum electrode collectively constitutes three-electrode system, use as auxiliary electrode, calomel electrode as corresponding reference electrode Cyclic voltammetry detects nifedipine content.
  2. 2. the method as described in claim 1, which is characterized in that in wherein step S50, buffer solution is phosphate buffer.
  3. 3. method as claimed in claim 2, which is characterized in that in wherein step S50, the pH of phosphate buffer is pH= 6.80。
  4. 4. method as claimed in claim 3, which is characterized in that in wherein step S70, nano cupric oxide modified glassy carbon electrode is swept Rate is retouched as 0.10V/s.
  5. 5. the method as described in claim 1, which is characterized in that wherein step S40 specifically comprises the following steps：
    S41, nifedipine sample treatment：The nifedipine tablets of certain mass are weighed, are smashed to pieces with mortar, are ground into powder Then grain adds in the absolute ethyl alcohol dissolution filter of certain volume, remove insoluble matter, forms transparent clear nifedipine sample Solution, it is In Shade, it is pipetted according to concentration needs for use；
    S42 prepares nifedipine mother liquor：It weighs nifedipine active compound to be placed in beaker, ethyl alcohol is added to dissolve, form 0.2 × 10- 2The nifedipine mother liquor of mol/L, it is In Shade spare.
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CN104698054A (en) * 2015-04-07 2015-06-10 天津理工大学 Non-enzymic glucose sensor of modified nanometer copper oxide screen-printed electrode
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