CN103439394A - Electrochemical method for detecting content of brown meat essence - Google Patents
Electrochemical method for detecting content of brown meat essence Download PDFInfo
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- CN103439394A CN103439394A CN2013104172619A CN201310417261A CN103439394A CN 103439394 A CN103439394 A CN 103439394A CN 2013104172619 A CN2013104172619 A CN 2013104172619A CN 201310417261 A CN201310417261 A CN 201310417261A CN 103439394 A CN103439394 A CN 103439394A
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Abstract
The invention discloses an electrochemical method for detecting content of brown meat essence. The electrochemical method comprises the steps of: 1, sanding a glassy carbon electrode by using abrasive paper of 1800#, 2000# and 4000#, cleaning with acetone, alcohol, a 10% NaOH solution, a 1:1 HNO3 solution and redistilled water, stoving; 2, scanning the glassy carbon electrode in 0.5mol/L H2SO4 at a scanning speed of 50mV.S<-1> in a range from -0.2V to 1.2V until reaching stable, stoving; 3, taking 10-20mL of 1-2mg/mL oxidized graphene water solution, adding NH3.H2O until the pH is 11.5, adding 5-10mL of 50mg/mL FeCl2 water solution, stirring, standing overnight, centrifuging, washing, stoving to obtain an Fe3O4/graphene compound material, preparing into a 1mg/mL solution, dispensing 3-5mu L of solution on the surface of the glassy carbon electrode to obtain an Fe3O4/graphene modified glassy carbon electrode; and 4, placing the Fe3O4/graphene modified glassy carbon electrode in a salbutamol sulfate solution, adding a B-R buffer solution with pH of 5-7, and detecting by using a differential pulse voltammetry, wherein the sampling width is 0.02s and the pulse period is 0.5s. The electrochemical method is simple and rapid, good in electrode stability, low in detection cost and good in reproducibility.
Description
Technical field
The invention belongs to the analyzing and testing field, relate to a kind of electrochemical method of clenbuterol hydrochloride content detection.Background technology
" clenbuterol hydrochloride " is that a class can promote the lean meat growth, suppress the medicine that fat meat is grown, and the material that can play at present this effect is the medicine that a class is called beta-stimulants (beta receptor activator).Mainly comprise the beta-stimulants such as clenobuterol hydrochloride, Ractopamine and salbutamol, bromine Boot sieve, bromine chlorine Boot sieve, Mabuterol.But after animal edible, can in internal organ and tissue, form the property accumulated residual, the mankind have eaten to be contained these medicine animal tissues and can produce serious toxic and side effect.So far in world wide existing number in thousand even ten thousand because eating the residual poisoning personnel of animal-derived food that clenbuterol hydrochloride is arranged.Show as after the edible residual livestock products that clenbuterol hydrochloride arranged of people that the excitation of muscle strengthens, systremma, long-term edible, cause in addition the possibility of chromosome aberration, thereby bring out malignant tumour, also may cause death.Therefore national governments have put into effect various rules and relevant policies about ban use of beta-stimulants in animal husbandry in succession.Because food variety is various, the matrix complexity, to the requirement for experiment condition harshness, so, set up a kind of simple, quick, believable detection method, and be applied to reality, be of great practical significance.At present the mensuration of clenbuterol hydrochloride in animal flesh in food and goods thereof mainly adopted to high performance liquid chromatography, gas-technology such as matter coupling, but these detection methods must have, and high-grade detecting instrument, sample pre-treatments are complicated, detection time is long, analysis cost is high, can't realize the quick Site Detection of a large amount of samples and be difficult to popularize, therefore application is restricted.The present invention Fe
3o
4/ graphene modified glass-carbon electrode, carry out accordingly the analysis of salbutamol sulfate and measure.The advantage such as that the method has is easy, reliable and stable, sensitivity is high.
Summary of the invention
The object of the present invention is to provide a kind of electrochemical method that detects clenbuterol hydrochloride content, it is to use Fe
3o
4/ graphene modified glass-carbon electrode, carry out the detection to a kind of salbutamol sulfate in clenbuterol hydrochloride accordingly.
With Fe
3o
4/ graphene modified glass-carbon electrode comprises the following steps the detection of clenbuterol hydrochloride:
(1) glass-carbon electrode is used respectively 1800#, 2000#, and 4000# abrasive paper for metallograph sanding and polishing, then use respectively acetone, ethanol, 10%NaOH solution, the HNO of 1:1
3solution, redistilled water cleans, dry for standby.
(2) the pretreated glass-carbon electrode of process (1) obtained is with 50mVS
-1sweep speed at 0.5mol/LH
2sO
4in-be scanned up between 0.2V-1.2V stablely, dry.
(3) get the graphite oxide aqueous solution of the 1-2 mg/mL of 10-20mL, dropwise drip NH
3﹒ H
2o, until pH is 11.5, more slowly drip 50mg/mL FeCl
2aqueous solution 5-10mL, stir, and it's 12 hours is past room temperature, centrifugal, and washing is dried and made Fe
3o
4/ graphene composite material.Prepared compound substance is configured to the solution of 1mg/mL, gets 3-5uL and drip and be applied to processed glass-carbon electrode surface, made Fe
3o
4/ graphene modified electrode.
(4) Fe prepared through (3)
3o
4/ graphene modified glass-carbon electrode is placed in the salbutamol sulfate solution of setting concentration, adds the pH scope between adding pH between the B-R of 5-7 buffer solution, adopts differential pulse voltammetry to detect it.The parameter of differential pulse voltammetry is: sweep limit: 0.4V-0.9V, current potential increment: 0.004V, amplitude: 0.05V, pulse width: 0.2s, sampling width: 0.02s, recurrence interval: 0.5s.
Adopt the beneficial effect of the technical program: compare the Fe that the present invention is prepared with the analyzing and testing of existing salbutamol sulfate
3o
4/ graphene modified glass-carbon electrode have the preparation method simple, fast, the good stability of electrode, can reuse, the advantage such as testing cost is low.Have by the analyzing and testing of this this modified electrode salbutamol sulfate that analysis speed is fast, sensing range wide, high repeatability and other advantages.
Analyzing and testing scope to salbutamol sulfate is: 1.0 * 10
-9mol/L-5.0 * 10
-5mol/L.
Measure 1 * 10
-6molL
-1salbutamol sulfate solution 10 times, its relative standard deviation is 2.7%.1 * 10
-6molL
-1salbutamol sulfate solution in, add respectively 100 times Clenbuterol, bricalin, dopamine, Ractopamine, ascorbic acid, urea, sucrose, glucose, lactose, talcum powder, starch, dolomol, dextrin and
l-halfcystine, measure salbutamol sulfate concentration, and result shows that its current-responsive deviation is less than 5%, and this display packing has selectivity preferably.
The salbutamol sulfate solution that the modified electrode respectively prepared by different batches is placed in same concentration is detected, the relative standard deviation of its oxidation peak current response (
n=5) be less than 2.9%, show that this modified electrode has reappearance preferably.Electrode is stored 7 days at 4 ℃, will after its taking-up, put into 1 * 10
-6molL
-1salbutamol sulfate solution, then press its Pulse Voltammetry oxidation peak current of determination of experimental method, found that this modified electrode storage after 2 months its electrochemical response changing value be less than 5%, show that this modified electrode has long-time stability preferably.
Embodiment
Glass-carbon electrode is used respectively 1800#, 2000#, and 4000# abrasive paper for metallograph sanding and polishing, then use respectively acetone, ethanol, 10%NaOH solution, the HNO of 1:1
3solution, redistilled water cleans, dry for standby.By this glass-carbon electrode with 50mVS
-1sweep speed at 0.5mol/LH
2sO
4in-be scanned up between 0.2V-1.2V stablely, dry.Get the graphite oxide aqueous solution of the 1-2 mg/mL of 10-20mL, dropwise drip NH
3﹒ H
2o, until pH is 11.5, more slowly drip FeCl
2(50mg/mL) aqueous solution 5-10mL, stir, and it's 12 hours is past room temperature, centrifugal, and washing is dried and made Fe
3o
4/ graphene composite material.Prepared compound substance is configured to the solution of 1mg/mL, gets 3-5uL and drip and be applied to processed glass-carbon electrode surface, made Fe
3o
4/ graphene modified electrode.
Fe by preparation
3o
4/ graphene modified electrode is placed in concentration between 1.0 * 10
-9mol/L-5.0 * 10
-5in the salbutamol sulfate solution of mol/L, add pH between the B-R of 5-7 buffer solution, adopt differential pulse voltammetry to detect it.The parameter of difference voltammetry is: sweep limit: 0.4V-0.9V, current potential increment: 0.004V, amplitude: 0.05V, pulse width: 0.2s, sampling width: 0.02s, recurrence interval: 0.5s.
Claims (2)
1. an electrochemical method that detects clenbuterol hydrochloride content, is characterized in that: with Fe
3o
4the detection of/graphene modified glass-carbon electrode to clenbuterol hydrochloride comprises the following steps: (1) glass-carbon electrode is used respectively 1800#, 2000#, and 4000# abrasive paper for metallograph sanding and polishing, then use respectively acetone, ethanol, 10%NaOH solution, the HNO of 1:1
3solution, redistilled water cleans, and dries; (2) the pretreated glass-carbon electrode of process above-mentioned (1) obtained is with 50mVS
-1sweep speed at 0.5mol/LH
2sO
4in-be scanned up between 0.2V-1.2V stablely, dry; (3) get the graphite oxide aqueous solution 10-20mL of 1-2 mg/mL, dropwise drip NH
3﹒ H
2o, until pH is 11.5, more slowly drip 50mg/mL FeCl
2aqueous solution 5-10mL, stir, and it's 12 hours is past room temperature, centrifugal, and washing is dried and made Fe
3o
4/ graphene composite material; Prepared compound substance is configured to the solution of 1mg/mL, gets 3-5uL and drip and be applied to processed glass-carbon electrode surface, made Fe
3o
4/ graphene modified glass-carbon electrode; (4) through Fe
3o
4/ graphene modified glass-carbon electrode is placed in the salbutamol sulfate solution of setting concentration, add the pH scope between adding pH between the B-R of 5-7 buffer solution, adopt differential pulse voltammetry to detect it, the sweep limit of differential pulse voltammetry: 0.4V-0.9V, current potential increment: 0.004V, amplitude: 0.05V, pulse width: 0.2s, sampling width: 0.02s, the recurrence interval: 0.5s.
2. according to the electrochemical method of the described detection clenbuterol hydrochloride of claim 1 content, it is characterized in that: described setting concentration is by Fe
3o
4/ graphene modified electrode is placed in concentration between 1.0 * 10
-9mol/L-5.0 * 10
-5in the salbutamol sulfate solution of mol/L.
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| CN103439394B CN103439394B (en) | 2015-04-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034766A (en) * | 2014-06-20 | 2014-09-10 | 遵义师范学院 | Preparation method and application of electrochemical transducer for fast detecting Sudan red in food |
| CN113466300A (en) * | 2021-07-16 | 2021-10-01 | 福建师范大学 | Preparation method of graphene modified silica sol loaded salbutamol antibody sensor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915792A (en) * | 2010-08-13 | 2010-12-15 | 上海交通大学 | Preparation method of electrochemical immunosensor for detecting salbutamol quickly |
| CN103063833A (en) * | 2013-01-21 | 2013-04-24 | 济南大学 | Preparation method and application of unmarked immunosensor for rapidly detecting clenbuterol |
-
2013
- 2013-09-13 CN CN201310417261.9A patent/CN103439394B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915792A (en) * | 2010-08-13 | 2010-12-15 | 上海交通大学 | Preparation method of electrochemical immunosensor for detecting salbutamol quickly |
| CN103063833A (en) * | 2013-01-21 | 2013-04-24 | 济南大学 | Preparation method and application of unmarked immunosensor for rapidly detecting clenbuterol |
Non-Patent Citations (2)
| Title |
|---|
| XIAOYUN LIN ET AL: ""A novel electrochemical sensor for the analysis of -agonists: The poly(acid chrome blue K)/graphene oxide-nafion/glassy carbon electrode"", 《JOURNAL OF HAZARDOUS MATERIALS》, 10 June 2013 (2013-06-10), pages 508 - 517, XP028693784, DOI: doi:10.1016/j.jhazmat.2013.06.004 * |
| 罗宿星等: ""硫酸特布他林在石墨烯修饰电极上的电化学行为及应用分析"", 《表面技术》, vol. 42, no. 3, 30 June 2013 (2013-06-30), pages 112 - 115 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034766A (en) * | 2014-06-20 | 2014-09-10 | 遵义师范学院 | Preparation method and application of electrochemical transducer for fast detecting Sudan red in food |
| CN113466300A (en) * | 2021-07-16 | 2021-10-01 | 福建师范大学 | Preparation method of graphene modified silica sol loaded salbutamol antibody sensor |
| CN113466300B (en) * | 2021-07-16 | 2023-04-14 | 福建师范大学 | Preparation method of graphene modified silica sol loaded salbutamol antibody sensor |
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