CN106872544A - A kind of preparation method of poly- methyl blue/acetylene black composite modified glassy carbon electrode and its application in paracetamol is determined - Google Patents
A kind of preparation method of poly- methyl blue/acetylene black composite modified glassy carbon electrode and its application in paracetamol is determined Download PDFInfo
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Abstract
The present invention is prepared for the poly- complex film modified glass-carbon electrode of methyl blue/acetylene black using electrodeposition process and drop-coating, electrochemical behavior of the paracetamol (PCT) on modified electrode is have studied with cyclic voltammetry (CV), test result indicate that, redox of the modified electrode for PCT has good electrocatalysis characteristic, relative to bare electrode and poly- methyl blue acetylene black modified electrode, oxidation peak currents of the PCT on poly- methyl blue/acetylene black modified glassy carbon electrode is significantly improved, determined using differential pulse voltammetry (DPV), PCT is 2.0 × 10‑6~0.4 × 10‑3With oxidation peak current in good linear relationship in mol/L concentration ranges, coefficient correlation is respectively 0.992, and PCT detections are limited to 1.0 × 10 when signal to noise ratio is 3‑6mol/L。
Description
Technical field
The invention belongs to chemically modified electrode technical field, and in particular to a kind of poly- composite modified glass of methyl blue/acetylene black
The preparation method of carbon electrode and its application in paracetamol is determined.
Background technology
Chemically modified electrode is one of Disciplinary Frontiers of current most active electrochemistry and Electroanalytical Chemistry.It is in electrode
Surface carries out MOLECULE DESIGN, electrode is had certain specific chemistry and electrochemical properties.The species of current modified electrode is a lot,
Such as organic molecule, metal nanoparticle (Nanoparticles, NPs) and thin polymer film etc..Wherein, thin polymer film is used
To electrode surface modify the polymer thin film modified electrode of preparation, because type of polymer is various, performance as dressing agent
Stabilization, concentration containing electric activity center is high, there is three-dimensional available potential field, and method of modifying is simple, quickly grows, in electrification
The fields such as, sensor are widely used.
The chemical entitled paracetamol (acetaminophen) of paracetamol (Paracetamol, abbreviation PCT), is virtue
The amide-type medicine of ring contraposition substitution, there is antipyretic, analgesic activity, has an impact to blood platelet and clotting mechanism.It is clinically main to use
Pain in cat fever, arthralgia, neuralgia and antimigraine, carcinomas pain and Post operation etc..Recently, domestic and international some research institutions
Constantly find the new role of paracetamol, such as long-term taking can reduce danger, attenuating miocardial infarction that women has ovarian cancer and in
The incidence of disease of wind.In recent years in succession it has been reported that paracetamol has turned into the wind of the diseases such as asthma, anaphylactia and apoplexy
Dangerous factor, therefore the extensive interest of people is caused to the measure of paracetamol content, set up it is accurate, quick, sensitively flutter heat
Breath pain content analysis method has important practical significance in terms of clinical medicine and pharmaceutical research.At present, the survey of paracetamol
Determining method mainly has AAS, high performance liquid chromatography, capillary electrophoresis, fluorescence method and portable injection chemiluminescence
Method etc..Either these methods use the instrument of complex and expensive, or need to carry out time-consuming more sample pretreatment process.
The content of the invention
It is an object of the invention to provide it is a kind of with sensitivity it is high, instrument is simple, the measure of the low advantage of analysis cost is flutterred
The method of heat breath pain.
To achieve the above object, present invention employs biological organic dyestuff methyl blue (Methyl Blue, MB) and nanometer material
Material acetylene black (Acetylene black, ACET) carrys out modified glassy carbon electrode, has prepared that poly- methyl blue/acetylene black is compound to repair
Decorations glass-carbon electrode.
The preparation method of the poly- methyl blue/acetylene black composite modified glassy carbon electrode is as follows：1. by solid-to-liquid ratio 0.1~
0.3mg: 1mL is added in distilled water acetylene black, and ultrasonic disperse is uniform, obtains acetylene black suspension；2. glass-carbon electrode is thrown
Light, is cleaned by ultrasonic in absolute ethyl alcohol and distilled water successively, is then cleaned with distilled water, dry for standby；3. acetylene black is suspended
Drop is added in the glassy carbon electrode surface after 2. step is processed, and drying obtains acetylene black modified glassy carbon electrode；4. acetylene black is modified
Glass-carbon electrode is placed on containing poly- methyl blue PBS cushioning liquid, and be polymerized 15~25min under the constant potential of 1.6V, obtains poly- methyl
Indigo plant/acetylene black composite modified glassy carbon electrode.
Preferably, the preparation method of the poly- methyl blue/acetylene black composite modified glassy carbon electrode is as follows：1. by 0.2mg second
Acetylene black is added in 1mL distilled water, ultrasonic disperse 120min, obtains acetylene black suspension；2. glass-carbon electrode is used 0.3 μ successively
M, 0.05 μm of alumina powder are polished in minute surface on chamois leather, each in absolute ethyl alcohol and distilled water successively to be cleaned by ultrasonic 5min,
Then cleaned with distilled water, infrared lamp dry for standby；3. the acetylene black hanging drop that 1. 6 μ L steps are prepared is taken with microsyringe
The glassy carbon electrode surface after 2. step is processed is added in, drying obtains acetylene black modified glassy carbon electrode under infrared lamp；4. by acetylene black
Modified glassy carbon electrode is placed on containing 5.0 × 10-3In the PBS cushioning liquid of the pH=9.0 of the poly- methyl blues of mol/L, in the perseverance of 1.6V
Be polymerized 20min under current potential, obtains poly- methyl blue/acetylene black composite modified glassy carbon electrode.
Described poly- methyl blue/acetylene black composite modified glassy carbon electrode is as follows to the assay method of paracetamol：In room temperature
Under, respectively with poly- methyl blue/acetylene black composite modified glassy carbon electrode as working electrode, saturated calomel electrode is reference electrode, platinum
Electrode is auxiliary electrode, and differential pulse volt is carried out in the ABS cushioning liquid of the paracetamol of the pH=5.0 containing various concentrations
Peace scanning, records various concentrations paracetamol oxidation peak current value, as a result shows paracetamol concentration 2.0 × 10-6~4.0 ×
10-4In the range of mol/L, its concentration has good linear relationship, drawing curve with oxidation peak current value, and linear equation is
The unit of I=-1.506-0.0396C, I is μm ol/L for the unit of μ A, C, and linearly dependent coefficient R=0.991, detection is limited to
1.0×10-6Mol/L, S/N=3；The oxidation peak current value of solution to be measured is determined, linear equation I=-1.506- is substituted into
The unit of 0.0396C, I is μm ol/L for the unit of μ A, C, calculates the content of paracetamol in solution to be measured.
The beneficial effect comprise that：Present invention cyclic voltammetry is polymerized system after glassy carbon electrode surface first drips Tu
For poly- methyl blue/acetylene black modified electrode, paracetamol electrochemical behavior on this electrode is have studied, establish measure trace
Measure the new method of paracetamol.This tests the measure for paracetamol, and detection limit has 2 up to 1.0 μm of ol/L, the range of linearity
The order of magnitude, and stability, service life are higher.
Brief description of the drawings
Fig. 1 is differential pulse of the paracetamol of various concentrations on poly- methyl blue/acetylene black composite modified glassy carbon electrode
Graph of a relation between volt-ampere curve and the oxidation peak current and its concentration of paracetamol；
Fig. 2 is the cyclic voltammogram of different modifying electrode；
Fig. 3 is the AC impedance figure of Different electrodes.
Specific embodiment
Embodiment 1
The preparation method of poly- methyl blue/acetylene black composite modified glassy carbon electrode is as follows：1. 0.2mg acetylene blacks are added into 1mL to steam
In distilled water, ultrasonic disperse 120min obtains acetylene black suspension；2. by glass-carbon electrode (effective diameter 3mm) successively with 0.3 μm,
0.05 μm of alumina powder is polished in minute surface on chamois leather, each in absolute ethyl alcohol and distilled water successively to be cleaned by ultrasonic 5min, so
Cleaned with distilled water afterwards, infrared lamp dry for standby；3. the acetylene black suspension dropwise addition that 1. 6 μ L steps are prepared is taken with microsyringe
Glassy carbon electrode surface after 2. step is processed, drying obtains acetylene black modified glassy carbon electrode (ACET/GCE) under infrared lamp；④
Acetylene black modified glassy carbon electrode is placed on containing 5.0 × 10-3PBS cushioning liquid (the phosphoric acid of the pH=9.0 of the poly- methyl blues of mol/L
Buffer salt solution) in, be polymerized 20min under the constant potential of 1.6V, obtains poly- methyl blue/acetylene black composite modified glassy carbon electrode.
It is measured that (between -0.2~1.2V, sweep speed is to paracetamol using differential pulse voltammetry (DPV)
100mV/s is circulated voltammetric scan；Between 0.2~0.8V, sweep speed is swept for 100mV/s carries out differential pulse voltammetry
Retouch).
Specific assay method is as follows：At room temperature, respectively with poly- methyl blue/acetylene black composite modified glassy carbon electrode as work
Electrode, saturated calomel electrode is reference electrode, and platinum electrode is auxiliary electrode, containing various concentrations (2,15,30,60,100,
200、300、400μmol/L；Carried out in the ABS cushioning liquid (acetate buffer solution) of the paracetamol of pH=5.0 a-h)
Differential pulse voltammetry is scanned, and various concentrations paracetamol oxidation peak current value is recorded, as shown in figure 1, as a result showing paracetamol
Concentration is 2.0 × 10-6~4.0 × 10-4In the range of mol/L, its concentration has good linear relationship with oxidation peak current value,
As shown in figure 1, linear equation is I=-1.506-0.0396C, the unit of I is μm ol/ for the unit of μ A, C to drawing curve
L, linearly dependent coefficient R=0.991, detection are limited to 1.0 × 10-6Mol/L, S/N=3.Determine the oxidation peak current of solution to be measured
Value, substitutes into the unit of linear equation I=-1.506-0.0396C, I for the unit of μ A, C is μm ol/L, you can calculate solution to be measured
The content of middle paracetamol.
Electrochemical catalysis behavior of the paracetamol on Different electrodes (sweep speed is 100mV/s)
In containing 500 μm of ABS acetate buffer solutions of the 0.1mol/L of the paracetamol of ol/L (pH=5.0), have studied
Cycle voltammetry behavior of the paracetamol on Different electrodes, as a result as shown in Figure 2.As seen from Figure 2, paracetamol is being ground
Study carefully and an obvious oxidation peak occurs during the anodic scan on electrode, but during reverse scan, do not observe corresponding
Reduction peak, the electrode process for showing paracetamol is irreversible oxidizing process.With glass-carbon electrode bare electrode (compared with curve a),
In poly- methyl blue modified electrode, (peak current on curve b) has increased slightly paracetamol, and peak row improves (the glass carbon for cleaning up
Electrode carries out above-mentioned steps voltolisation closing operation 4. and can be prepared by poly- methyl blue modification electricity instead of the glass-carbon electrode that acetylene black is modified
Pole)；In acetylene black modified glassy carbon electrode, (peak current on curve c) also has increased slightly, and peak shape improves；Paracetamol is in poly- methyl
(peak current on curve d) reaches maximum to indigo plant/acetylene black composite modified glassy carbon electrode.As can be seen here, due to methyl blue polymer
With the collective effect of nanometer acetylene black, electrode surface property is improved, there is provided more reaction site, increase electrode has
Validity response area, and the electron transport rate of paracetamol and electrode surface is accelerated, it is effectively improved to paracetamol
Electrocatalysis.
Influence of the Different electrodes to AC impedance
Containing 1mmol/LFe (CN)6 3-/4-In 0.1mol/LKCl solution, the impedance (Fig. 3) of different modifying electrode is have studied.
As seen from Figure 3, with bare electrode (compared with curve a), poly- methyl blue modified electrode (impedance on curve b) is significantly reduced,
And acetylene black modified glassy carbon electrode (impedance on curve c) is slightly reduced.In poly- methyl blue/acetylene black compound modification glass carbon electricity
(the impedance ratio bare electrode on curve d) is small, and it is bigger than poly- methyl blue modified electrode for pole.
In summary, poly- methyl blue and acetylene black modified glassy carbon electrode are made electrochemical sensor and can be used for paracetamol
Sensitive determination.Due to the excellent electric conductivity of poly- methyl blue and filming performance and the excellent electric conductivity of nano material acetylene black
And catalytic performance, make the modified electrode that there is good catalytic performance, table for the electrochemical redox process of paracetamol
Now for its oxidation peak current significantly improves and aoxidize the negative shifting of spike potential.Test result indicate that, the electrochemical sensor has stabilization
Good, the easy preparation of property and low cost and other advantages.The analysis method set up has sensitivity and the range of linearity wide high, can be used for
The measure of the middle paracetamol content such as medicament.
Claims (4)
1. a kind of preparation method of poly- methyl blue/acetylene black composite modified glassy carbon electrode, it is characterised in that comprise the following steps：①
Acetylene black is added in distilled water by solid-to-liquid ratio 0.1~0.3mg: 1mL, ultrasonic disperse is uniform, obtains acetylene black suspension；②
Glass-carbon electrode is polished, is cleaned by ultrasonic in absolute ethyl alcohol and distilled water successively, then cleaned with distilled water, dry for standby；③
Acetylene black hanging drop is added in the glassy carbon electrode surface after 2. step is processed, drying obtains acetylene black modified glassy carbon electrode；④
During acetylene black modified glassy carbon electrode is placed on containing poly- methyl blue PBS cushioning liquid, under the constant potential of 1.6V be polymerized 15~
25min, obtains poly- methyl blue/acetylene black composite modified glassy carbon electrode.
2. as claimed in claim 1 poly- methyl blue/acetylene black composite modified glassy carbon electrode preparation method, it is characterised in that including
Following steps：1. 0.2mg acetylene blacks are added in 1mL distilled water, ultrasonic disperse 120min obtains acetylene black suspension；②
Glass-carbon electrode is polished with 0.3 μm, 0.05 μm of alumina powder on chamois leather successively, it is each super in absolute ethyl alcohol and distilled water successively
Sound cleans 5min, is then cleaned with distilled water, infrared lamp dry for standby；3. the acetylene black hanging drop that 1. 6 μ L steps are prepared is taken
The glassy carbon electrode surface after 2. step is processed is added in, drying obtains acetylene black modified glassy carbon electrode under infrared lamp；4. by acetylene black
Modified glassy carbon electrode is placed on containing 5.0 × 10-3In the PBS cushioning liquid of the pH=9.0 of the poly- methyl blues of mol/L, in the perseverance of 1.6V
Be polymerized 20min under current potential, obtains poly- methyl blue/acetylene black composite modified glassy carbon electrode.
3. poly- methyl blue/acetylene black composite modified glassy carbon electrode that prepared by the preparation method of claim 1 or 2 flutters hot breath in measure
Application in pain.
4. application as claimed in claim 3, it is characterised in that comprise the following steps：At room temperature, respectively with poly- methyl blue/second
Acetylene black composite modified glassy carbon electrode is working electrode, and saturated calomel electrode is reference electrode, and platinum electrode is auxiliary electrode, is being contained
Differential pulse voltammetry (DPV) scanning is carried out in the ABS cushioning liquid of the paracetamol of the pH=5.0 of various concentrations, record is different
Concentration paracetamol oxidation peak current value, as a result shows paracetamol concentration 2.0 × 10-6~4.0 × 10-4Mol/L scopes
Interior, its concentration has good linear relationship with oxidation peak current value, and drawing curve, linear equation is I=-1.506-
The unit of 0.0396C, I is μm ol/L, linearly dependent coefficient R=0.991 for the unit of μ A, C, and detection is limited to 1.0 × 10-6mol/
L, S/N=3；The oxidation peak current value of solution to be measured is determined, unit the μ A, C of linear equation I=-1.506-0.0396C, I is substituted into
Unit be μm ol/L, calculate the content of paracetamol in solution to be measured.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107576715A (en) * | 2017-09-17 | 2018-01-12 | 桂林理工大学 | A kind of method that concentration of benzoic acid is detected using modified glassy carbon electrode |
| CN109060907A (en) * | 2018-07-06 | 2018-12-21 | 信阳师范学院 | Application of the poly- complex film modified glass-carbon electrode of gold/acetylene black in detection hydroquinone |
| CN109164083A (en) * | 2018-11-13 | 2019-01-08 | 青岛大学 | Based on copper nano-cluster/carbon dots/arginine complex paracetamol ratio fluorescent sensor preparation method |
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| US20090202880A1 (en) * | 2007-11-01 | 2009-08-13 | Yi Ge | Electrochemical mediators |
| CN106556633A (en) * | 2016-11-10 | 2017-04-05 | 无锡市明盛强力风机有限公司 | A kind of method of modifying of glass-carbon electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20090202880A1 (en) * | 2007-11-01 | 2009-08-13 | Yi Ge | Electrochemical mediators |
| CN106556633A (en) * | 2016-11-10 | 2017-04-05 | 无锡市明盛强力风机有限公司 | A kind of method of modifying of glass-carbon electrode |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107576715A (en) * | 2017-09-17 | 2018-01-12 | 桂林理工大学 | A kind of method that concentration of benzoic acid is detected using modified glassy carbon electrode |
| CN107576715B (en) * | 2017-09-17 | 2019-11-26 | 桂林理工大学 | A method of concentration of benzoic acid is detected using modified glassy carbon electrode |
| CN109060907A (en) * | 2018-07-06 | 2018-12-21 | 信阳师范学院 | Application of the poly- complex film modified glass-carbon electrode of gold/acetylene black in detection hydroquinone |
| CN109164083A (en) * | 2018-11-13 | 2019-01-08 | 青岛大学 | Based on copper nano-cluster/carbon dots/arginine complex paracetamol ratio fluorescent sensor preparation method |
| US10983057B2 (en) | 2018-11-13 | 2021-04-20 | Qingdao University | Method for preparing a ratiometric fluorescent sensor for paracetamol based on a copper nanoclusters-carbon dots-arginine composite |
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