CN104316588A - Flavonoids compound sensor, and preparation method and application thereof - Google Patents
Flavonoids compound sensor, and preparation method and application thereof Download PDFInfo
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- CN104316588A CN104316588A CN201410636546.6A CN201410636546A CN104316588A CN 104316588 A CN104316588 A CN 104316588A CN 201410636546 A CN201410636546 A CN 201410636546A CN 104316588 A CN104316588 A CN 104316588A
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Abstract
The invention discloses a favonoids compound sensor, and a preparation method and application thereof. The method comprises the steps of polishing the cross section of a carbon fiber micro-disk electrode, performing ultrasonic cleaning on the polished carbon fiber micro-disk electrode, then immersing the cross section of the carbon fiber micro-disk electrode into a chloroauric acid solution, keeping the electric precipitation electric potential to be minus 0.2 V and the electric precipitation time to be 10 to 30 s, taking out the electrode and drying the electrode, immersing the electrode into mixed solution of graphene oxide and multiwalled carbon nanotube for 5 to 15 s, drying the electrode, reducing the graphene oxide on the electrode, keeping the reduction potential to be minus 0.7 to minus 1.2 V and the electroreduction time to be 150 to 370 s so as to obtain the favonoids compound sensor. The favonoids compound sensor has the advantages that the linearity range of the electrode is wide, the sensitivity is high, the response speed is high, and the sensor can be applied to one or more separable favonoids compound in plant detection through a capillary electrophoresis electrochemistry method.
Description
Technical field
The invention belongs to technical field of electroanalytical chemistry detection, particularly a kind of flavone compound sensor and its preparation method and application.
Background technology
Chemically modified electrode be 20 century 70s, of to grow up mid-term emerging, be also the Disciplinary Frontiers of current most active galvanochemistry and Electroanalytical Chemistry.Chemically modified electrode carries out various modification on conductor or semi-conducting electrode, thus give electrode certain special character, the shortcomings such as the overpotential occurred when overcoming unmodified determination of electrode is higher, sensitivity is low, are especially widely used in analytical chemistry field in the preparation of biology sensor.
Conventional chemically modified electrode has carbon magma microelectrode, metal and nonmetallic nano-particle modified microelectrode, Surface film Modified ultramicroelectrode, powder microelectrode, enzyme electrode etc.Gold stable chemical nature, golden nanometer particle shows excellent electro catalytic activity due to small-size effect etc., and it shows application prospect widely in chemically modified electrode research.Graphene modified electrode is attached to electrode surface in modes such as absorption, dipping by Graphene by Graphene, thus improve the character of primary electrode, expands the range of application of electrode.Carbon nano-tube is since being found by the mankind, and be just described as following material, be one of Disciplinary Frontiers of international scientific in recent years always.It is one of study hotspot becoming the world with the structure of its uniqueness, characteristic electron, mechanical property and chemical stability.
Flavone compound plays an important role in the development and growth process of plant.Flavone compound is the chemistry " health products " of coronary heart disease, angiocardiopathy, anti-inflammatory and antalgic and antitumor activity, and its oxidation resistance also has certain inhibiting effect to cataract and chloasma.Flavone compound plays a part more and more important at medical domain, and electroanalysis chemical process has the advantages such as selectivity is good, highly sensitive, easy to operate, analysis speed is fast, has development and application prospect widely in the detection of flavone compound.
At present, report that detecting the detection method of flavone compound has ultraviolet spectrophotometry, infra-red sepectrometry, fluorescence spectrophotometry, thin layer chromatography scanning and LC-MS-MS, liquid chromatography etc.As: M.NavarroEscamilla, F.RodenasSanz, H.Li, S.A.
b.Yang b, G.K.Bonn, C.W.Huck.Talanta, 2013,114:304-310, the infra-red sepectrometry that the document uses.Carvalho, JM; Leandro, KC; Da Silva, AR; Aucelio, RQ.Selective determination of rutin by fluorescence attenuation of the CdS-2-mercaptopropionic acid nanocrystal probe.Analytical Letters, 2013,46:207-224, the document uses fluorimetry.But these methods have the shortcomings such as complicated operation, cost be higher.Capillary electrophoresis with electrochemical detection only needs to measure electric current usually, and this method is simple to operate, and has high sensitivity and high selectivity to electroactive material, is therefore also commonly used to detect flavone compound.
Summary of the invention
The object of this invention is to provide a kind of flavone compound sensor and preparation method thereof.Another object of the present invention is to provide the application of this kind of flavone compound sensor in capillary electrophoresis amperometric detects.
The technical scheme that the present invention takes is:
A preparation method for flavone compound sensor, comprises step as follows:
(1) by level and smooth for the polishing of carbon fiber microdisk electrode xsect, ultrasonic cleaning, dry, be immersed in chlorauric acid solution electro-deposition, electro-deposition current potential is at-0.1 ~-0.7V, and electrodeposition time is 5-60s, dries, and obtains gold nano carbon fiber microdisk electrode;
(2) by gold nano carbon fiber microdisk electrode, be immersed in 5s ~ 60s in the mixed solution of graphene oxide and multi-walled carbon nano-tubes, dry, obtain the microdisk electrode after dipping;
(3) the graphene oxide electroreduction will the microdisk electrode after dipping be stained with, reduction potential is at-0.2 ~-1.2V, and electroreduction time 30 ~ 500s, obtains flavone compound sensor;
Described graphene oxide and the mass ratio of multi-walled carbon nano-tubes are: 0.5-1:1-5.
In step (1), described ultrasonic cleaning is each ultrasonic 3-5min in intermediate water, absolute ethyl alcohol, intermediate water respectively.
The flavone compound sensor (as Fig. 1) that said method is obtained
The present invention obtains flavone compound sensor and detects the application in flavone compound and the application as capillary analysis instrument detecting device at capillary electrophoresis electrochemical.
Capillary electrophoresis electrochemical detects qualitative, the quantitative measurement that can be used for flavone compound astragalin in plant and medicine, rutin and Quercetin, by transit time and go out the peak area at peak can to Flavonoids from Plants, as astragalin, rutin and Quercetin carry out quantitative and qualitative analysis.Kapillary respectively cleans 5min with the borate buffer solution of the NaOH solution of 0.2mol/L, intermediate water, 10-50mmol/L before every use all respectively.The positive pole of high-voltage power supply is inserted in the sample inlet pool of the borate buffer solution filling 10-50mmol/L together with the sample introduction end of kapillary, the endpiece of kapillary is fixed on detection cell, working electrode is fixed on three-dimensional manipulating instrument, regulate three-dimensional manipulating instrument, working electrode is made to align with the endpiece of separation capillary under the microscope, sample inlet pool is connected with the negative pole of high-voltage power supply, and high-voltage power supply forms loop with the kapillary being full of damping fluid, forms the piece-rate system of capillary zone electrophoresis.Open CHI810C electrochemical analyser, connect contrast electrode and to electrode, cover shielded box, regulate high-voltage power supply to 18kV, after baseline is steady, regulate high-voltage power supply to 5kV, sample introduction desired concn flavonoid matter sample 10s, then recall to 18kV by high-voltage power supply, running experiment also records electrophoretogram.
Experimental result shows sensor electrode of the present invention for common flavone compound astragalin, rutin and Quercetin respectively 5.0 × 10
-7~ 3.7 × 10
-4mol/L, 5.0 × 10
-7~ 3.2 × 10
-4mol/L and 1.0 × 10
-6~ 3.0 × 10
-4mol/L internal linear relation is good, and its linearly dependent coefficient is respectively 0.9993,0.9991,0.9989.At optimum conditions, this electrode is respectively 5.0 × 10 for the detectability of astragalin, rutin and Quercetin
-7mol/L, 5.0 × 10
-7mol/L and 1.0 × 10
-6mol/L, detectability is lower compared with the prior art, and the detectability of this electrode is low, highly sensitive as can be seen here, using the detecting device of this electrode as Capillary Electrophoresis, achieves the qualitative and quantitative analysis of flavone compound in plant and medicine.
Advantageous Effects of the present invention:
1. the sensor surface that the present invention obtains has a lot of fold, this configuration increases the specific surface area of this modified electrode, thus catalytic activity point is rolled up, facilitate the transfer rate of electronics, improve electroactive material especially flavone compound as astragalin, rutin and Quercetin response sensitivity (as Fig. 2).
2. the range of linearity of sensor electrode of the present invention is wide, highly sensitive, fast response time.Because flavone compound has similar structure, so the character of flavone compound has certain similarity.Therefore this sensor can be used for one or more the separable flavone compounds in capillary electrophoresis electrochemical method detection plant and medicine.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of sensor electrode of the present invention.
Fig. 2 is the electrophoretic image of astragalin, rutin and Quercetin gained in capillary electrophoresis amperometric detects in the present invention.
Embodiment
Further illustrate below in conjunction with embodiment.
The preparation of embodiment 1 flavone compound sensor
Before carrying out chemical modification, the surface of carbon fiber electrode must process totally, and concrete grammar is, it is carefully polished on abrasive paper for metallograph, makes electrode surface smooth, then each ultrasonic 5min in intermediate water, ethanol, intermediate water successively, at room temperature dries.By the xsect that carbon fiber microdisk electrode is polished, be immersed in chlorauric acid solution, electro-deposition current potential is at-0.2V, and electrodeposition time is 10s, and taking-up is dried.Before graphene oxide multi-walled carbon nano-tubes mixed solution is tested at every turn, be first placed in ultrasonic cleaning instrument ultrasonic disperse 30min.For producing gold nano-graphene oxide multi-walled carbon nano-tubes Modified carbon fiber electrode, the xsect of carbon fiber electrode is dipped in 10s in graphene oxide carbon nano-tube mixed solution by us, carbon fiber electrode is avoided to immerse in graphene oxide multi-walled carbon nano-tubes mixed solution too dark, in order to avoid make electrode activity surface expand.Take out electrode, dry under room temperature.Then the gold dried-graphene oxide Multiwalled Carbon Nanotubes Modified Electrode is put into the phosphate buffered solution of the 0.1mol/L containing pH 4.0, electro-deposition 250s under-0.9V voltage.After taking-up, rinse well with intermediate water, naturally dry, namely obtained flavone compound sensor.
The preparation of embodiment 2 flavone compound sensor
Before carrying out chemical modification, the surface of carbon fiber electrode must process totally, and concrete grammar is, it is carefully polished on abrasive paper for metallograph, makes electrode surface smooth, then each ultrasonic 5min in intermediate water, ethanol, intermediate water successively, at room temperature dries.By the xsect that carbon fiber microdisk electrode is polished, be immersed in chlorauric acid solution, electro-deposition current potential is at-0.2V, and electrodeposition time is 20s, and taking-up is dried.Before graphene oxide multi-walled carbon nano-tubes mixed solution is tested at every turn, be first placed in ultrasonic cleaning instrument ultrasonic disperse 30min.For producing gold nano-graphene oxide multi-walled carbon nano-tubes Modified carbon fiber electrode, the xsect of carbon fiber electrode is dipped in 10s in graphene oxide carbon nano-tube mixed solution by us, carbon fiber electrode is avoided to immerse in graphene oxide multi-walled carbon nano-tubes mixed solution too dark, in order to avoid make electrode activity surface expand.Take out electrode, dry under room temperature.Then the gold dried-graphene oxide Multiwalled Carbon Nanotubes Modified Electrode is put into the phosphate buffered solution of the 0.1mol/L containing pH 4.0, electro-deposition 200s under-1.0V voltage.After taking-up, rinse well with intermediate water, naturally dry, namely obtained flavone compound sensor.
The preparation of embodiment 3 flavone compound sensor
Before carrying out chemical modification, the surface of carbon fiber electrode must process totally, and concrete grammar is, it is carefully polished on abrasive paper for metallograph, makes electrode surface smooth, then each ultrasonic 5min in intermediate water, ethanol, intermediate water successively, at room temperature dries.By the xsect that carbon fiber microdisk electrode is polished, be immersed in chlorauric acid solution, electro-deposition current potential is at-0.5V, and electrodeposition time is 30s, and taking-up is dried.Before graphene oxide multi-walled carbon nano-tubes mixed solution is tested at every turn, be first placed in ultrasonic cleaning instrument ultrasonic disperse 30min.For producing gold nano-graphene oxide multi-walled carbon nano-tubes Modified carbon fiber electrode, the xsect of carbon fiber electrode is dipped in 30s in graphene oxide carbon nano-tube mixed solution by us, carbon fiber electrode is avoided to immerse in graphene oxide multi-walled carbon nano-tubes mixed solution too dark, in order to avoid make electrode activity surface expand.Take out electrode, dry under room temperature.Then the gold dried-graphene oxide Multiwalled Carbon Nanotubes Modified Electrode is put into the phosphate buffered solution of the 0.1mol/L containing pH 4.0, electroreduction 300s under-0.8V voltage.After taking-up, rinse well with intermediate water, naturally dry, namely obtained flavone compound sensor.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (6)
1. a preparation method for flavone compound sensor, is characterized in that, comprises step as follows:
(1) by level and smooth for the polishing of carbon fiber microdisk electrode xsect, ultrasonic cleaning, dry, be immersed in chlorauric acid solution electro-deposition, electro-deposition current potential is at-0.2 ~-0.7V, and electrodeposition time is 10-30s, dries, and obtains gold nano carbon fiber microdisk electrode;
(2) by gold nano carbon fiber microdisk electrode, be immersed in 5 ~ 15s in the mixed solution of graphene oxide and multi-walled carbon nano-tubes, dry, obtain the microdisk electrode after dipping;
(3) the graphene oxide electroreduction will the microdisk electrode after dipping be stained with, reduction potential is at-0.7 ~-1.2V, and electroreduction time 150 ~ 370s, obtains flavone compound sensor;
Described graphene oxide and the mass ratio of multi-walled carbon nano-tubes are: 0.5-1:1-5.
2. the preparation method of a kind of flavone compound sensor according to claim 1, is characterized in that, in step (1), described ultrasonic cleaning is each ultrasonic 3-5min in intermediate water, absolute ethyl alcohol, intermediate water respectively.
3. the preparation method of a kind of flavone compound sensor according to claim 1, is characterized in that, in step (3), described electroreduction current potential is-0.9V, and the electroreduction time is 250s.
4. the flavone compound sensor that the arbitrary described method of claim 1-3 is obtained.
5. flavone compound sensor according to claim 4 detects the application in flavone compound at capillary electrophoresis electrochemical.
6. flavone compound sensor according to claim 4 is in the application of preparation capillary analysis instrument detecting device.
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| CN105259225A (en) * | 2015-11-20 | 2016-01-20 | 重庆市中药研究院 | Method and special electrochemical transducer for rapid selective detection of luteolin |
| CN105277601A (en) * | 2015-11-13 | 2016-01-27 | 重庆市中药研究院 | Method and special electrochemical detector for electrochemical detection of baicalein |
| CN105628774A (en) * | 2016-01-12 | 2016-06-01 | 山东师范大学 | Graphene modified electrode for amperometric detection of capillary electrophoresis and preparation method thereof |
| CN108998011A (en) * | 2018-07-16 | 2018-12-14 | 辽宁大学 | Carbon quantum dot with polyion fluorescence response and preparation method thereof and the application in Plant Taxonomy |
| CN114166908A (en) * | 2021-12-13 | 2022-03-11 | 中北大学 | Preparation method and detection method of tea polyphenol and component analysis electrochemical sensor thereof |
| CN114674906A (en) * | 2022-03-14 | 2022-06-28 | 云南中烟工业有限责任公司 | Method for simultaneously detecting nicotine and phenolic substances in tobacco by capillary electrophoresis amperometry |
| CN117025200A (en) * | 2023-10-08 | 2023-11-10 | 吉林农业大学 | Biosensor for detecting flavonoid compounds and preparation method |
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- 2014-11-12 CN CN201410636546.6A patent/CN104316588B/en not_active Expired - Fee Related
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| CN105277601A (en) * | 2015-11-13 | 2016-01-27 | 重庆市中药研究院 | Method and special electrochemical detector for electrochemical detection of baicalein |
| CN105259225A (en) * | 2015-11-20 | 2016-01-20 | 重庆市中药研究院 | Method and special electrochemical transducer for rapid selective detection of luteolin |
| CN105259225B (en) * | 2015-11-20 | 2019-03-19 | 重庆市中药研究院 | A kind of luteolin fast selective detection method and its dedicated electrochemical sensor |
| CN105628774A (en) * | 2016-01-12 | 2016-06-01 | 山东师范大学 | Graphene modified electrode for amperometric detection of capillary electrophoresis and preparation method thereof |
| CN105628774B (en) * | 2016-01-12 | 2018-06-08 | 山东师范大学 | A kind of capillary electrophoresis amperometric detection graphene modified electrode and preparation method thereof |
| CN108998011A (en) * | 2018-07-16 | 2018-12-14 | 辽宁大学 | Carbon quantum dot with polyion fluorescence response and preparation method thereof and the application in Plant Taxonomy |
| CN108998011B (en) * | 2018-07-16 | 2021-04-13 | 辽宁大学 | Application of carbon quantum dots with multi-ion fluorescence response in plant taxonomy |
| CN114166908A (en) * | 2021-12-13 | 2022-03-11 | 中北大学 | Preparation method and detection method of tea polyphenol and component analysis electrochemical sensor thereof |
| CN114166908B (en) * | 2021-12-13 | 2024-04-02 | 中北大学 | Preparation method and detection method of tea polyphenol and component analysis electrochemical sensor thereof |
| CN114674906A (en) * | 2022-03-14 | 2022-06-28 | 云南中烟工业有限责任公司 | Method for simultaneously detecting nicotine and phenolic substances in tobacco by capillary electrophoresis amperometry |
| CN117025200A (en) * | 2023-10-08 | 2023-11-10 | 吉林农业大学 | Biosensor for detecting flavonoid compounds and preparation method |
| CN117025200B (en) * | 2023-10-08 | 2023-12-22 | 吉林农业大学 | Biosensor for detecting flavonoid compounds and preparation method |
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