CN104101634A - Method for preparing electrochemical sensor based on synthetic zinc oxide nano-rod - Google Patents
Method for preparing electrochemical sensor based on synthetic zinc oxide nano-rod Download PDFInfo
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- CN104101634A CN104101634A CN201410368116.0A CN201410368116A CN104101634A CN 104101634 A CN104101634 A CN 104101634A CN 201410368116 A CN201410368116 A CN 201410368116A CN 104101634 A CN104101634 A CN 104101634A
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Abstract
The invention relates to a method for preparing an electrochemical sensor based on both a synthetic zinc oxide nano-rod and a novel 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid modified carbon paste electrode. The electrochemical sensor is used for detecting levodopa with existence of carbidopa, is simple to operate, high in response speed, good in repeatability and low in price and has a lower detection limit; during detection, the time-consuming extraction step is not needed, influence from pH is avoided, reaction with oxygen does not happen and innocuity is ensured; therefore, the electrochemical sensor is simple, accurate, precise, low-price and quick in detection, and has a relatively good application prospect in clinical practice that carbidopa and levodopa are detected at the same time.
Description
Technical field
The present invention relates to a kind of preparation method of electrochemical sensor, relate in particular to a kind of preparation method of the electrochemical sensor detecting for the lower levodopa of carbidopa existence based on synthesizing zinc oxide nanometer rods.
Background technology
Parkinsonian's Etiological is dopamine neuron serious degradation contained in brain, and dopamine can not be directly used in treatment, because it cannot pass through blood-brain barrier.The presoma levodopa of dopamine can pass through blood-brain barrier, at brain, by dopamine decarboxylase, is transformed into dopamine, so levodopa is widely used in parkinsonian clinical treatment.
If levodopa too high levels, can be metabolized to excessive dopamine, thereby have side effects, as nauseating, vomiting, attitude low blood pressure etc., more seriously may cause mental illness.Levodopa is combined with the carbidopa that can suppress DOP Adecarboxylase and pass through blood-brain barrier, dopamine can be controlled to rational concentration, thereby reduces spinoff.Therefore,, in order to reach better medical effect and to reduce toxicity, the control of levodopa and carbidopa content in medicine is just become to extremely important.
Levodopa and carbidopa structural similarity, separation difficulty, therefore the method simultaneously detecting for the two is also less, in biological sample and medicine, the detection of levodopa and carbidopa has at present: spectrophotometric method, high efficiency liquid phase color method and chemiluminescence etc., but every kind of method all can run into the use from cost, selectivity, organic solvent, complicated preparation of samples program and long restriction analysis time.
Summary of the invention
The present invention has prepared a kind of electrochemical sensor of the New Carbon Paste Electrode based on zinc paste (ZnO) nanometer rods and 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid modified, has the detection of lower levodopa for carbidopa.
Zinc paste (ZnO) is a kind of wide semiconductor that can be with (3.37eV) and wurtzite structure that has, and is widely used in the fields such as sensing, optoelectronic device, photo-detector, aurora transmitter, catalysis and photoelectronic device.ZnO also can synthesize the nanometer film that contains multiple one-dimentional structure (as nanobelt, nanorod and nanowire) simultaneously, has high specific surface area and good mechanical stability, is suitable for very much electrode and sensor.The present invention utilizes ZnO nanorod and 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid to carry out modification to glassy carbon electrode, thereby obtains a kind of novel electrochemical sensor, has the content of lower levodopa in order to detect carbidopa.
Step of the present invention is as follows:
(1) ZnO nanorod is synthetic: the Zn (NO that first prepares 200～400mL0.01～0.02mol/L
3)
26H
2o solution packs in pressure bottle with hexamethylenetetramine (HMT) simultaneously, and fiber is immersed in pressure bottle solution, at 60～80 ℃, heats 6～12h, with the rotating speed centrifuging of 20000～50000rpm, goes out sediment.
(2) 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid synthesizing: the Ortho-Aminophenol that is 1:1～4:1 by mol ratio and the acid of 4-bromstyrol and 5～10g catalyzer tetrakis triphenylphosphine palladium (Pd (PPh
3)
4) join in the conical bottle of 100～300mL, add with liquor capacity than being the dimethyl acetamide of 1:10～1:8 (DMA), potpourri maintains 24～48h being heated to 50～80 ℃, has reacted rear cooling 10～30min, and Pd (PPh is collected in vacuum filtration
3)
4methenyl choloride is joined in potpourri to filtering catalyst again, again primary products is carried out to recrystallization in isopropyl alcohol and methenyl choloride (40:60～50:50, volume ratio v/v), obtain pure 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid.
(3) preparation of modified electrode: by 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid, powdered graphite and ZnO nanorod mortar hand mix, mass ratio is 1:60:100～1:80:200, paraffin oil is joined and in said mixture, mixes 30～80min, until form homogeneous pastel, pastel is filled into a glass tube (diameter 1.5～3mm, length 8～12cm) end, inserting a copper cash provides and electrically contacts, can obtain based on zinc paste (ZnO) nanometer rods and 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid modified New Carbon Paste Electrode.
The present invention has prepared a kind of electrochemical sensor of the New Carbon Paste Electrode based on zinc paste (ZnO) nanometer rods and 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid modified, has the detection of lower levodopa for carbidopa.When the electrochemical sensor the present invention relates to detects carbidopa and levodopa at the same time, simple to operate, response rapidly, favorable repeatability, cheap, there is lower detectability; In testing process, do not need extraction step consuming time, not affected by pH, do not react with oxygen and nontoxic; Be a kind of simply, accurately, accurately, at a low price, detect electrochemical sensor rapidly, in the clinical practice that carbidopa and levodopa detect simultaneously, there is good application prospect.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with implementing, the invention will be further described.
The electrochemical sensor preparation method who exists lower levodopa to detect for carbidopa based on synthesizing zinc oxide nanometer rods, its step is as follows:
(1) ZnO nanorod is synthetic: the Zn (NO that first prepares 300mL0.015mol/L
3)
26H
2o solution packs in pressure bottle with hexamethylenetetramine (HMT) simultaneously, and fiber is immersed in pressure bottle solution, at 60 ℃, heats 12h, with the rotating speed centrifuging of 30000rpm, goes out sediment.
(2) 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid synthesizing: by 1.09g (10mmol) Ortho-Aminophenol, 2.27g (10mmol) 4-bromstyrol acid and 5g tetrakis triphenylphosphine palladium (Pd (PPh
3)
4) join in the conical bottle of 200mL, then add 20mL dimethyl acetamide (DMA), be heated to 80 ℃ and maintain 24h, reacted rear cooling 20min, Pd (PPh is collected in vacuum filtration
3)
4; Methenyl choloride is joined in potpourri to filtering catalyst again, again to primary products at isopropyl alcohol and methenyl choloride (40:60, volume ratio v/v) in, carry out recrystallization, obtain pure 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid, productive rate is 64%.
(3) preparation of modified electrode: by 0.03g5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid, 1.8g powdered graphite and 0.3gZnO nanometer rods mortar hand mix, paraffin oil is joined in said mixture and mixes 50min until form homogeneous pastel, pastel is filled into a glass tube (diameter 2mm, length 12cm) end, inserting a copper cash provides and electrically contacts, and can obtain based on zinc paste (ZnO) nanometer rods and 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid modified New Carbon Paste Electrode.
Claims (7)
1. a preparation method for the electrochemical sensor based on synthesizing zinc oxide nanometer rods, its step is as follows:
(1) ZnO nanorod is synthetic: the Zn (NO of preparation 200～400mL0.01～0.02mol/L
3)
26H
2o solution packs in pressure bottle with hexamethylenetetramine (HMT) simultaneously, and fiber is immersed in pressure bottle solution, at 60～80 ℃, heats 6～12h, with the rotating speed centrifuging of 20000～50000rpm, goes out sediment;
(2) 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid synthesizing: the Ortho-Aminophenol that is 1:1～4:1 by mol ratio and the acid of 4-bromstyrol and 5～10g catalyzer tetrakis triphenylphosphine palladium (Pd (PPh
3)
4) join in the conical bottle of 100～300mL, add with liquor capacity than being the dimethyl acetamide of 1:10～1:8 (DMA), be heated to 50～80 ℃ and maintain 24～48h, reacted rear cooling 10～30min, vacuum filtration collection Pd (PPh
3)
4methenyl choloride is joined in potpourri to filtering catalyst again, again primary products is carried out in isopropyl alcohol and methenyl choloride recrystallization, obtain pure 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid, the volume ratio of described isopropyl alcohol and methenyl choloride is 40:60～50:50;
(3) preparation of modified electrode: by 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid, powdered graphite and ZnO nanorod mortar hand mix, mass ratio is 1:60:100～1:80:200, paraffin oil is joined in said mixture and mixes 30～80min until form homogeneous pastel, pastel is filled into a glass tube (diameter 1.5～3mm, length 8～12cm) end, inserting a copper cash provides and electrically contacts, can obtain based on zinc paste (ZnO) nanometer rods and 5-(4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid modified New Carbon Paste Electrode.
2. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the described Zn (NO of step (1)
3)
26H
2the volume of O solution is 300mL, and concentration is 0.015mol/L.
3. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the described centrifuging rotating speed of step (1) is 30000rpm.
4. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the mol ratio of the described Ortho-Aminophenol of step (2) and the acid of 4-bromstyrol is 1:1.
5. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the volume ratio of the described isopropyl alcohol of step (2) and methenyl choloride is 40:60.
6. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the mass ratio of the described 5-of step (3) (4'-amino-3'-hydroxyl-diphenyl-4-alcohol)-acrylic acid, powdered graphite and ZnO nanorod is 1:60:100.
7. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the described diameter glass tube of step (3) is 2mm, and length is 12cm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271361A (en) * | 2015-10-28 | 2016-01-27 | 中国科学院上海微系统与信息技术研究所 | Preparation method of dendritic zinc oxide nanowire array |
| CN105424787A (en) * | 2015-11-20 | 2016-03-23 | 济南大学 | Preparation method of silk screen printing sensor for detecting tetracycline and oxytetracycline at same time |
| US11437606B2 (en) | 2019-02-26 | 2022-09-06 | King Fahd University Of Petroleum And Minerals | Fabrication of nanostructured palladium thin film for electrochemical detection of hydrazine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101526531A (en) * | 2009-03-20 | 2009-09-09 | 东南大学 | Method for immunoassay by utilizing zinc oxide quantum dots |
| CN103713019A (en) * | 2013-12-23 | 2014-04-09 | 浙江大学 | Zinc oxide/polypyrrole nano composite resistance-type film gas sensor and production method thereof |
-
2014
- 2014-07-29 CN CN201410368116.0A patent/CN104101634A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101526531A (en) * | 2009-03-20 | 2009-09-09 | 东南大学 | Method for immunoassay by utilizing zinc oxide quantum dots |
| CN103713019A (en) * | 2013-12-23 | 2014-04-09 | 浙江大学 | Zinc oxide/polypyrrole nano composite resistance-type film gas sensor and production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ELAHE MOLAAKBARI等: "Synthesis of ZnO nanorods and their application in the construction of a nanostructure-based electrochemical sensor for determination of levodopa in the presence of carbidopa", 《ANALYST》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271361A (en) * | 2015-10-28 | 2016-01-27 | 中国科学院上海微系统与信息技术研究所 | Preparation method of dendritic zinc oxide nanowire array |
| CN105271361B (en) * | 2015-10-28 | 2017-03-08 | 中国科学院上海微系统与信息技术研究所 | A kind of preparation method of dendroid zinc oxide nano-wire array |
| CN105424787A (en) * | 2015-11-20 | 2016-03-23 | 济南大学 | Preparation method of silk screen printing sensor for detecting tetracycline and oxytetracycline at same time |
| CN105424787B (en) * | 2015-11-20 | 2017-08-15 | 济南大学 | It is a kind of while detecting the preparation method of the silk-screen printing sensor of tetracycline and terramycin |
| US11437606B2 (en) | 2019-02-26 | 2022-09-06 | King Fahd University Of Petroleum And Minerals | Fabrication of nanostructured palladium thin film for electrochemical detection of hydrazine |
| US11677063B2 (en) | 2019-02-26 | 2023-06-13 | King Fahd University Of Petroleum And Minerals | Method for forming palladium thin film on glass substrate |
| US11705550B2 (en) | 2019-02-26 | 2023-07-18 | King Fahd University Of Petroleum And Minerals | Aerosol assisted deposition process for forming palladium thin film electrode |
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Application publication date: 20141015 |