CN109374706A - A method of trace carbadox is detected with the structure mesoporous carbon CMK-8 Direct Electrochemistry sensor of cube Ia3d - Google Patents
A method of trace carbadox is detected with the structure mesoporous carbon CMK-8 Direct Electrochemistry sensor of cube Ia3d Download PDFInfo
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- CN109374706A CN109374706A CN201811365014.8A CN201811365014A CN109374706A CN 109374706 A CN109374706 A CN 109374706A CN 201811365014 A CN201811365014 A CN 201811365014A CN 109374706 A CN109374706 A CN 109374706A
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Abstract
The present invention relates to a kind of methods with the structure mesoporous carbon CMK-8 Direct Electrochemistry sensor measurement trace carbadox of cube Ia3d.The present invention uses the structure mesoporous carbon CMK-8 modified glassy carbon electrode of cube Ia3d, and constructed sensor is used for the direct measurement of carbadox.When carbadox is in 0.5nM~500.0nM concentration range, the concentration of electrochemical signals response and carbadox is in good linear relationship, and method detection is limited to 74.4pM.Invention significantly improves the sensitivity of carbadox detection, and the detection of low concentration carbadox is easy to automate.
Description
Technical field
The invention belongs to new function materials, electrochemical sensing detection technique field, are related to a kind of detection trace carbadox
Method, especially a kind of side with cube Ia3d structure mesoporous carbon CMK-8 Direct Electrochemistry sensor detection trace carbadox
Method.
Background technique
Carbadox (Carbadox, abbreviation CBX) is traditional quinoxaline drug, and such drug is the dynamic of chemical synthesis class
Object medicine dedicated has broad-spectrum antibacterial action and can promote the animal growths such as pig, chicken, ox, sheep, rabbit, and can be improved
The conversion ratio of feed, carbadox are widely used in the poultry farmings such as aquaculture and pig chicken.But many toxicology report displays
Carbadox has genetoxic, mutagenicity and carcinogenicity.It is added into feed, is had in vivo after animal edible obvious
Residual, has extremely serious harm to the health of human body.Therefore, even if China is such drug using big country, also have
Explicit stipulation is forbidden to use carbadox.But since it can increase the remarkable effects such as lean meat percentage, there are still disobeying orders to add service condition,
So it is particularly important to establish simple and effective carbadox detection method.
The report of carbadox detection method has more at present, mainly there is immunization, liquid chromatography, gas-chromatography-series connection
Mass spectrography, Liquid Chromatography-Tandem Mass Spectrometry etc..Also the national standard method of detection carbadox has been put into effect in China.Most common side
Method is Liquid Chromatography-Tandem Mass Spectrometry, but this method step when handling actual sample is complex, and wants to detecting instrument
Ask higher, it is not easy enough.Electrochemical Detection is efficiently quick, and selectivity is high, and high sensitivity, the requirement to instrument is relatively low, quilt
It is widely used in various detections, but the document report of electrochemical gaging carbadox is rarely seen.
Mesoporous material is porous material of the aperture between 2.0nm-50.0nm, and mesoporous carbon is the mesoporous material of a kind of non-silicon-based
Material.It has huge surface area (up to 2500m2/ g) and pore volume (2.25cm3/g).1999, Ryoo et al. was utilized
Template has synthesized order mesoporous carbon molecular sieve CMK-1 for the first time.Hereafter various ordered mesopore carbons are synthesized in succession.Orderly
Mesoporous carbon has some more excellent properties: cellular structure rule and high-sequential, aperture size narrowly distributing and in certain model
Enclose it is interior can regulate and control, specific surface area is very big, good conductivity, has good thermal stability and certain hydrothermal stability.Because of it
Function admirable, mesoporous carbon as electrode modified material in electrochemical catalysis and sensor using more and more extensive.Mesoporous carbon
CMK-3 be currently it is most widely used, and the structure mesoporous carbon CMK-8 of cube Ia3d then apply it is less.
Electrochemical sensor is a kind of sensor based on principle of electrochemical reaction come examination target object, it using electrode as
Sensor conversion element modifies material on the electrode as sensing element, the lewis' acid of sensing element and measured matter
It contacts and chemical reaction or variation occurs, conversion element is by this reaction or changes the direct or indirect electric signal that is converted into, and establishes
The relationship of the chemical quantities such as concentration, the ingredient of subject matter and output electric signal, to realize the device of the quantitative detection of subject matter.Electricity
Chemical sensor due to its with high sensitivity, selectivity it is good, easy to operate, detection quickly, easily micromation, can be in complication system
In monitor on-line the even superiority such as in-vivo analysis, oneself becomes research field very active in Electroanalytical Chemistry, and
Clinical examination, food and drugs analysis, environmental monitoring, in terms of be widely used.
Summary of the invention
To solve the deficiencies in the prior art, a kind of direct with the structure mesoporous carbon CMK-8 of cube Ia3d the invention reside in providing
The method that electrochemical sensor detects trace carbadox, this method are imitated using the amplification of the structure mesoporous carbon CMK-8 of cube Ia3d
It answers, can be used to detect trace carbadox in high sensitivity.
A kind of structure mesoporous carbon CMK-8 Direct Electrochemistry sensor detection trace kappa of cube Ia3d of the present invention
The method of oxygen, comprising the following steps:
A. the processing of gold electrode:
Gold electrode (Φ=3mm) is rinsed with secondary deionized water, then is thrown with 0.05 μm of gama-alumina polishing powder
Light polishing, washes again, dries spare；
B. the preparation of the structure mesoporous carbon CMK-8 dispersion liquid of cube Ia3d:
The structure mesoporous carbon CMK-8 powder of a certain amount of cube of Ia3d is accurately weighed, is dispersed with DMF, ultrasonic 1h is obtained
The mesoporous carbon dispersion liquid of finely dispersed 4mg/mL；
C. the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d:
Take the structure mesoporous carbon CMK-8 homogeneous dispersion drop coating of appropriate cube of Ia3d in through processed gold with microsyringe
It on electrode, is placed under infrared lamp and dries, dry in the air spare to room temperature；
D. the building of electrochemical sensor:
Modified electrode is placed in certain density Na3PO4It is scanned through differential pulse voltammetry to stabilization in buffer solution.With
Constant potential enrichment is carried out under 1000rpm magnetic agitation afterwards, potential region is -0.3V~0.7V, enrichment time 10-35min.
E. the detection of carbadox:
Electro-chemical test uses three-electrode system: working electrode is right for the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d
Electrode is hollow stud, and reference electrode is saturated calomel electrode；Electro-chemical test carries out in self-control electrolytic cell；Make electrolytic cell by oneself
Volume be 25mL, every time test when load electrolyte product be 20mL, be stirred using magnetic stirrer.Electrolyte is
Na3PO4Buffer solution adjusts pH value using NaOH, high pure nitrogen 5min is passed through before use sufficiently to eliminate dissolved oxygen therein.
The further feature of electrochemical sensor according to the present invention, cube Ia3d is structure mesoporous in the step C
The dosage of carbon CMK-8 dispersion liquid is 4 μ L.
The further feature of electrochemical sensor according to the present invention, in the step D, in the electrolytic cell
Na3PO4Buffer solution pH=7.0.
The further feature of electrochemical sensor according to the present invention, in the step D, the accumulating potential is
0.3V。
The further feature of electrochemical sensor according to the present invention, in the step D, the enrichment time is
25min。
Electrochemical sensor of the present invention for detecting trace carbadox overcomes prior art in detection kappa
It is excessively cumbersome that there are methods when oxygen, and the shortcomings such as step complexity preferably improve the sensitivity of detection, for trace kappa
The detection of oxygen is easy to automate.
Detailed description of the invention
Fig. 1 is the differentiated pulse volt-ampere curve of Different electrodes, in figure, (a) bare electrode, and (b) the structure mesoporous carbon of cube Ia3d
CMK-8 modified electrode.Insertion figure is the enlarged drawing of bare electrode.
Fig. 2 is sensor standard absorption curve of the present invention.
Fig. 3 is the chart of the selectivity of sensor of the present invention.It is the substance being added on horizontal axis, extremely by a left side in figure
The right side is followed successively by the chaff interferents such as urea, uric acid, hypoxanthine, ascorbic acid, inosine.
Specific embodiment
Embodiment 1: of the present invention for detecting the building of the electrochemical sensor of micro carbadox
A kind of structure mesoporous carbon CMK-8 Direct Electrochemistry sensor detection trace kappa of cube Ia3d of the present invention
The method of oxygen the following steps are included:
(1) processing of gold electrode:
Gold electrode (Φ=3mm) is rinsed with secondary deionized water, then is thrown with 0.05 μm of gama-alumina polishing powder
Light polishing, washes again, dries spare；
(2) preparation of the structure mesoporous carbon CMK-8 dispersion liquid of cube Ia3d:
The structure mesoporous carbon CMK-8 powder of a certain amount of cube of Ia3d is accurately weighed, is dispersed with DMF, ultrasonic 1h is obtained
The mesoporous carbon dispersion liquid of finely dispersed 4mg/mL.
(3) the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d:
Take the structure mesoporous carbon CMK-8 homogeneous dispersion drop coating of appropriate cube of Ia3d in through processed gold with microsyringe
It on electrode, is placed under infrared lamp and dries, dry in the air spare to room temperature.
(4) building of electrochemical sensor:
Modified electrode is placed in certain density Na3PO4It is scanned through differential pulse voltammetry to stabilization in buffer solution.With
Constant potential enrichment is carried out under 1000rpm magnetic agitation afterwards, potential region is -0.3V~0.7V, enrichment time 10-35min.
(5) detection of carbadox:
Electro-chemical test uses three-electrode system: working electrode is right for the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d
Electrode is hollow stud, and reference electrode is saturated calomel electrode.Electro-chemical test carries out in self-control electrolytic cell.Make electrolytic cell by oneself
Volume be 25mL, every time test when load electrolyte product be 20mL, be stirred using magnetic stirrer.Electrolyte is
Na3PO4Buffer solution adjusts pH value using NaOH, high pure nitrogen 5min is passed through before use sufficiently to eliminate dissolved oxygen therein.
Embodiment 2: the electrochemical sensor differentiated pulse volt-ampere characterization of the present invention for detecting trace carbadox
Using Differential Pulse Voltammetry observation carbadox in bare electrode, the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d
On electrochemical reaction.As shown in Figure 1, on bare electrode (curve a), the peak current of 2 μM of carbadox are 0.46 μ A, and vertical
(curve b), up to 233.4 μ A are caused, (curve a), opposite bare electrode have peak current under the modification of the square structure mesoporous carbon CMK-8 of Ia3d
507 times of peak current amplification.And it is evident that baseline of the baseline of curve b obviously compared with curve a moves down by Fig. 2, this is illustrated
CMK-8 has huge specific surface area, can effectively increase signal.
Embodiment 3: the range of linearity and detection limit are tested
It, can based on the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d to the extremely strong electro-catalysis effect of kappa oxygen electric reduction
To establish the hypersensitive electrochemical detection method of carbadox.When carbadox is in 0.1nM~500.0nM concentration range, electrochemistry
Signal response and the concentration of carbadox are in good linear relationship (referring to fig. 2), equation of linear regression be-I (μ A)=
0.503 × C (nmol/L) -0.128, R=0.997, detection are limited to 74.4pM.Invention significantly improves the spirits of carbadox detection
Sensitivity is easy to automate for the detection of low concentration carbadox.
Embodiment 4: the influence of chaff interferent
Selectivity tests this experiment by comparing sensor peak current ratio (I/I0) interference experiment is carried out, as shown in figure 3, working as
When kappa oxygen concentration is 100nM, the chaff interferents such as urea, uric acid, hypoxanthine, ascorbic acid, inosine of 100 times of concentration are equal to its
It is noiseless.
Embodiment 5: actual sample measurement
After treatment by actual sample, its extracting solution is taken, electrochemical gaging is carried out, measurement result is shown in Table 1.It can by table 1
The rate of recovery of perception method is 89.75%~105.38%, relative standard deviation 9.87-4.23%.
Table 1: actual sample mark-on testing result (n=5).
| Spiked levels (nM) | The rate of recovery (%) | RSD |
| 50 | 89.75 | 9.87 |
| 100 | 105.38 | 5.81 |
| 200 | 98.7 | 4.23 |
Claims (5)
1. a kind of method with the structure mesoporous carbon CMK-8 Direct Electrochemistry sensor detection trace carbadox of cube Ia3d, special
Sign is, comprising the following steps:
A. the processing of gold electrode:
Gold electrode (Φ=3mm) is rinsed with secondary deionized water, then carries out polishing with 0.05 μm of gama-alumina polishing powder and beats
Mill, washes again, dries spare；
B. the preparation of the structure mesoporous carbon CMK-8 dispersion liquid of cube Ia3d:
The structure mesoporous carbon CMK-8 powder of a certain amount of cube of Ia3d is accurately weighed, is dispersed with DMF, ultrasonic 1h, must be dispersed
The mesoporous carbon dispersion liquid of even 4mg/mL；
C. the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d:
Take the structure mesoporous carbon CMK-8 homogeneous dispersion drop coating of appropriate cube of Ia3d in through processed gold electrode with microsyringe
On, it is placed under infrared lamp and dries, dry in the air spare to room temperature；
D. the building of electrochemical sensor:
Modified electrode is placed in certain density Na3PO4It is scanned through differential pulse voltammetry to stabilization in buffer solution.Then exist
Constant potential enrichment is carried out under 1000rpm magnetic agitation, potential region is -0.3V~0.7V, enrichment time 10-35min；
E. the detection of carbadox:
Electro-chemical test uses three-electrode system: working electrode is the structure mesoporous carbon CMK-8 modified electrode of cube Ia3d, to electrode
For hollow stud, reference electrode is saturated calomel electrode；Electro-chemical test carries out in self-control electrolytic cell；Make the appearance of electrolytic cell by oneself
Product is 25mL, and loading electrolyte product when test every time is 20mL, is stirred using magnetic stirrer；Electrolyte is Na3PO4
Buffer solution adjusts pH value using NaOH, high pure nitrogen 5min is passed through before use sufficiently to eliminate dissolved oxygen therein.
2. according to the method described in claim 1, it is characterized by: in the step C, the described cube of structure mesoporous carbon of Ia3d
The dosage of CMK-8 dispersion liquid is 4 μ L.
3. according to the method described in claim 1, it is characterized by: in the step D, Na in the electrolytic cell3PO4It buffers molten
The pH of liquid is 7.0.
4. according to the method described in claim 1, it is characterized by: the accumulating potential is 0.3V in the step D.
5. according to the method described in claim 1, it is characterized by: the enrichment time is 25min in the step D.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811365014.8A CN109374706B (en) | 2018-11-16 | 2018-11-16 | Method for detecting trace amount of carbalkoxy by using cubic Ia3d structure mesoporous carbon CMK-8 direct electrochemical sensor |
| JP2019166741A JP6684381B1 (en) | 2018-11-16 | 2019-09-13 | Method for detecting trace carbadox using direct electrochemical sensor with mesoporous carbon CMK-8 having cubic Ia3d structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811365014.8A CN109374706B (en) | 2018-11-16 | 2018-11-16 | Method for detecting trace amount of carbalkoxy by using cubic Ia3d structure mesoporous carbon CMK-8 direct electrochemical sensor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988074A (en) * | 2019-12-20 | 2020-04-10 | 肇庆学院 | CoCu @ cubic Ia3d structure mesoporous carbon electrochemical sensor and application thereof in detection of trace cyadox |
| CN110988071A (en) * | 2019-12-20 | 2020-04-10 | 肇庆学院 | Application of graphitized hydroxyl multi-walled carbon nanotube @ cubic Ia3d structured mesoporous carbon electrochemical sensor in detection of thiamethoxam |
| CN113340958A (en) * | 2021-06-23 | 2021-09-03 | 肇庆学院 | Working electrode of high-sensitivity quercetin electrochemical sensor and application thereof |
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| CN110988071A (en) * | 2019-12-20 | 2020-04-10 | 肇庆学院 | Application of graphitized hydroxyl multi-walled carbon nanotube @ cubic Ia3d structured mesoporous carbon electrochemical sensor in detection of thiamethoxam |
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| CN113340958A (en) * | 2021-06-23 | 2021-09-03 | 肇庆学院 | Working electrode of high-sensitivity quercetin electrochemical sensor and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6684381B1 (en) | 2020-04-22 |
| CN109374706B (en) | 2020-06-30 |
| JP2020085889A (en) | 2020-06-04 |
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