CN103675054A - Electrolytic tank and method for detecting dopamine - Google Patents
Electrolytic tank and method for detecting dopamine Download PDFInfo
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- CN103675054A CN103675054A CN201210361734.3A CN201210361734A CN103675054A CN 103675054 A CN103675054 A CN 103675054A CN 201210361734 A CN201210361734 A CN 201210361734A CN 103675054 A CN103675054 A CN 103675054A
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- solution pool
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- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229960003638 dopamine Drugs 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 47
- 239000004005 microsphere Substances 0.000 claims abstract description 20
- 238000005859 coupling reaction Methods 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 239000007853 buffer solution Substances 0.000 claims abstract description 10
- 238000001903 differential pulse voltammetry Methods 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 238000007639 printing Methods 0.000 claims description 14
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 7
- 229910052753 mercury Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 239000007974 sodium acetate buffer Substances 0.000 claims description 4
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000012190 activator Substances 0.000 claims description 2
- 150000001718 carbodiimides Chemical class 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000007420 reactivation Effects 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 230000005389 magnetism Effects 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000000903 blocking effect Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000026058 directional locomotion Effects 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 230000001960 triggered effect Effects 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000008878 coupling Effects 0.000 description 7
- 238000010168 coupling process Methods 0.000 description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000000872 buffer Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 238000007885 magnetic separation Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000003411 electrode reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 description 1
- 208000018737 Parkinson disease Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 150000003943 catecholamines Chemical class 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000002858 neurotransmitter agent Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 201000000980 schizophrenia Diseases 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses an electrolytic tank and a method for detecting dopamine. The electrolytic tank comprises an upper part and a lower part, wherein the upper part comprises an inverted circular truncated cone-shaped tank body and a tank cover provided with a hole; the lower part comprises a cylindrical tank bottom; a piece of magnet with strong magnetism is arranged in a concave hole in the middle of the bottom of the tank; the upper part and the lower part are fixedly locked by a blocking position and screws; a rubber pad is arranged at the part at which the upper part is connected with the lower part; the tank body in the electrolytic tank is made from polytetrafluoroethylene. In a buffer system, dopamine solution to be detected is triggered by an activating agent so as to have a coupling reaction with magnetic microspheres; the reaction product is enriched on the surface of a printed carbon electrode under the applied magnetic field of the electrolytic tank; the peak current is detected by a differential pulse voltammetry; a linear relation is established by the peak current and the standard sample concentration; the concentration of the sample to be detected can be obtained according to the established linear relation. The magnetism can be generated by the magnetic microspheres under the action of the applied magnetic field of the electrolytic tank, and the magnetic microspheres carry out directional movement and are enriched on the surface of a working electrode, so that the detection sensitivity is improved.
Description
Technical field
The present invention relates to a kind of testing equipment and detection method thereof of electrochemical field, more specifically relate to a kind of electrolytic cell for detection of dopamine and method thereof.
Background technology
Dopamine is the Catecholamines Neurotransmitters in Blood being present in mammalian central nervous system, and the change of its amount can cause some important diseases as schizophrenia and Parkinson's disease.During at present with electrochemical method determining dopamine, because the overpotential of dopamine on solid electrode is high, electrode reaction is slow, and its electrochemical reaction product is easily adsorbed in electrode surface, has caused electrode surface passivation, and detection sensitivity reduces.
Summary of the invention
According to an aspect of the present invention, a kind of electrolytic cell for detection of dopamine is provided, comprise that Chi Tiji is positioned over the working electrode of Chi Tizhong, to electrode and contrast electrode, pond body comprises Chi Gai, at the bottom of solution pool and pond, cover strip hole, pond, solution pool is inverted round stage shape, at the bottom of pond, be cylindrical, at the bottom of pond, in the middle of bottom, be provided with shrinkage pool, magnet is housed in shrinkage pool, magnet lower end is provided with spring, working electrode crosses at junction at the bottom of solution pool and pond, the working portion of working electrode is towards solution pool, electrode and contrast electrode are inserted in the hole of Chi Gai, working portion to electrode and contrast electrode enters in solution pool.
In some embodiments, at the bottom of solution pool and pond, by fastened by screw, at the bottom of solution pool and pond, junction is provided with rubber blanket.
In some embodiments, adopt teflon material at the bottom of solution pool, Chi Gai and pond, the bottom of electrolytic cell is coated with steel plate.
In some embodiments, working electrode is selected printing carbon electrode, and the carbon paste district of printing carbon electrode is circular, and electrode is selected to platinum electrode, and contrast electrode is selected mercury electrode.
A kind of detection method for detection of dopamine, comprise: under buffer system, by magnetic microsphere and the dopamine solution generation coupling reaction after activation, coupling reaction product is enriched in working electrode surface under magnetic field that electrolytic cell adds, by Differential Pulse Voltammetry, detect peak current, by peak current and standard specimen concentration, set up linear relationship, by set up linear relationship, draw testing sample concentration.
In some embodiments, working electrode is selected printing carbon electrode.
In some embodiments, buffer system is selected acetic acid-sodium-acetate buffer.
In some embodiments, the activator of using in reactivation process is carbodiimide.
The present invention is by after dopamine and magnetic microsphere coupling, under electrolytic cell externally-applied magnetic field condition, with the enrichment of printing carbon electrode, detect, the carbon paste district of printing carbon electrode is circular, make the rich region of coupled product larger, and magnetic microsphere has larger specific surface, thereby portability high density functional group and can high degree of dispersion characteristic in solution, under additional magnetic fields, soft magnetism polymer microsphere can produce magnetic, does surface that displacement is enriched in electrode to improve the sensitivity of its detection.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of electrolytic cell for detection of dopamine of the present invention;
Fig. 2 is the differentiated pulse voltammogram of an embodiment of a kind of electrolytic cell for detection of dopamine of the present invention and detection method thereof;
Fig. 3 is the time m-map of current of coupling reaction of the present invention after 5 minutes, 10 minutes, 20 minutes, 30 minutes, 40 minutes and 50 minutes;
Fig. 4 is that dopamine concentration of the present invention is respectively 1 * 10
-7mol/L, 2.5 * 10
-7mol/L, 5 * 10
-7mol/L, 7.5 * 10
-7mol/L, 10 * 10
-7concentration-the map of current being depicted as during mol/L.
Embodiment
Embodiment mono-
As shown in Figure 1, a kind of electrolytic cell for detection of dopamine, comprise pond body 1 and be positioned over the working electrode 2 of Chi Tizhong, to electrode 3 and contrast electrode 4.Pond body 1 comprises at the bottom of pond lid 11, solution pool 12 and pond 13.Pond lid 11 band circular holes, solution pool 12 is inverted round stage shape, at the bottom of pond, 13 is cylindrical.At the bottom of pond, in the middle of 13 bottoms, be provided with shrinkage pool, magnet 131 is housed in shrinkage pool, magnet 131 lower ends are provided with spring 132.Working electrode 2 crosses at 13 junctions at the bottom of solution pool 12 and pond, and the working portion of working electrode 2 is towards solution pool 12.Electrode 3 and contrast electrode 4 are inserted in the circular hole of pond lid 11, the working portion of electrode 3 and contrast electrode 4 is entered in solution pool.At the bottom of solution pool 12 and pond, 13 by fastened by screw, and at the bottom of solution pool 12 and pond, 13 junctions are provided with rubber blanket 5.In electrolytic cell, at the bottom of solution pool 12, pond lid 11 and pond, 13 material is teflon.The bottom of electrolytic cell is coated with steel plate 6.Working electrode 2 is selected printing carbon electrode, and the carbon paste district of printing carbon electrode is circular, and contrast electrode 4 is selected mercury electrode, and electrode 3 is selected to platinum electrode.
First the ethanol water ultrasonic cleaning that is 90% by solution pool by mass concentration 30 minutes, then ultrapure water clean after at 80 ℃ dry for standby.Working electrode is faced up and inserts at the bottom of solution pool 12 and pond 13 junction, and adjust working electrode 2 positions and make working portion completely from 13 exposing at the bottom of pond, lock screw; Finally, dopamine solution to be measured is poured in solution pool 12, by electrode 3 and contrast electrode 4 are put in the circular hole of pond lid 11, made the perform region of electrode 3 and contrast electrode 4 enter in solution pool 12.Connecting galvanochemistry platform tests.
The activation of carboxyl magnetic microsphere: measure 50uL carboxyl magnetic microsphere emulsion (solid content 5～20g/L, surface carboxyl amount >=0.25mmol/g, mean grain size 60nm) in test tube, after adding 5mL NaAc_HAc buffer solution (PH=4.6) dilution to shake up, adding 0.05mL concentration is 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride activation of 100mg/L, after 30 minutes, with ultrapure water, clean magnetic-adsorption activation products, abandoning supernatant, use respectively again 2mL hac buffer (pH=3.6) washing 3 times, finally in test tube, add 5mL hac buffer (pH=3.6).
Get 10uL concentration and be 5mmol/L dopamine for hydrochloric acid solution NaAc_HAc buffer solution (pH=3.6) in the volumetric flask of 50mL constant volume dilution for after 1ppm.The dopamine solution coupling reaction that carboxyl magnetic microsphere solution after 5mL is activated and 5mL concentration are 1ppm is after 50 minutes, magnetic microsphere is carried out to magnetic separation, with deionized water washing 3 times, then the magnetic microsphere after coupling is transferred in electrolytic cell, the NaAc_HAc buffer solution (pH=3.6) that the 10mL concentration of take is 0.05mol/L is electrolytic solution, magnetic microsphere quick adsorption under the externally-applied magnetic field of the magnet 131 of electrolytic cell after coupling is to the surface of printing electrode, and puts into subsequently mercury electrode and platinum electrode and carries out Differential Pulse Voltammetry and detect.Location parameter: initial potential is-0.1V, final current potential 0.7V, sweep velocity is 4mV/s, and pulse height is 50mV, and the sampling time is 20 seconds, and pulse width is 60 milliseconds, and the recurrence interval is 2000 milliseconds, and be 2 seconds rest time.
Conventional Differential Pulse Voltammetry test: getting 10uL concentration is that 5mmol/L dopamine hydrochloric acid solution dilutes for after 1ppm with 0.05mol/L NaAc_HAc buffer solution (pH=3.6) constant volume in the volumetric flask of 50mL, pours in 100mL small beaker.Printing carbon electrode, mercury electrode and platinum electrode are put into solution and carry out Differential Pulse Voltammetry.Location parameter: nitrogen continues to pass into 5 minutes comes deoxygenation, initial potential to be-0.1V, final current potential 0.7V, sweep velocity is 4mV/s, and pulse height is 50mV, and the sampling time is 20 seconds, pulse width is 60 milliseconds, and the recurrence interval is 2000 milliseconds, and be 2 seconds rest time.
As shown in Figure 2, directly measure peak current=1.158 * 10 of dopamine
-6a, peak current=1.069 * 10 of magnetic field measuring dopamine after coupling
-5a.Under externally-applied magnetic field, coupled product is enriched in electrode surface, makes oxidation peak current amplify 9.2 times, and spike potential is negative to be moved, and has improved the sensitivity of electrode reaction.
Embodiment bis-
Get 10uL concentration and be 5mmol/L dopamine for hydrochloric acid solution hac buffer (pH=3.6) in the volumetric flask of 50mL constant volume dilution for after 1ppm.The dopamine solution coupling reaction that magnetic microsphere solution after 5mL is activated and 5mL concentration are 1ppm is after 5 minutes, magnetic microsphere is carried out to magnetic separation, with deionized water washing 3 times, then microballoon is transferred in electrolytic cell of the present invention, acetic acid sodium acetate buffer solution (pH=3.6) 10ml of 0.05mol/L of take is electrolytic solution, magnetic microsphere quick adsorption under the externally-applied magnetic field of electrolytic cell after coupling is to the surface of printing electrode, and puts into subsequently mercury electrode and platinum electrode and carries out Differential Pulse Voltammetry and detect.Location parameter: initial potential is-0.1V, final current potential 0.7V, sweep velocity is 4mV/s, and pulse height is 50mV, and the sampling time is 20 seconds, and pulse width is 60 milliseconds, and the recurrence interval is 2000 milliseconds, and be 2 seconds rest time.The in the situation that of each parameter constant, the time that changes coupling reaction is respectively reacts for 10 minutes, 20 minutes, 30 minutes, 40 minutes and 50 minutes.
As shown in Figure 3, Fig. 3 has provided the time m-map of current of coupling reaction after 5 minutes, 10 minutes, 20 minutes, 30 minutes, 40 minutes and 50 minutes, as seen from Figure 3, coupling reaction 30 minutes, it is stable that oxidation peak current reaches.
Get 10uL concentration and be 5mmol/L dopamine for hydrochloric acid solution NaAc_HAc buffer solution (pH=3.6) in dilution, be 0.5 * 10
-7after the concentration of mol/L.By the 5mL magnetic microsphere solution after activation, be 0.5 * 10 with concentration successively
-7the dopamine solution coupling reaction of mol/L is after 30 minutes, magnetic microsphere is carried out to magnetic separation, with deionized water washing 3 times, then microballoon is transferred in electrolytic cell, acetic acid-sodium acetate buffer solution (pH=3.6) 10mL of 0.05mol/L of take is electrolytic solution, magnetic microsphere quick adsorption under the externally-applied magnetic field of electrolytic cell after coupling is to the surface of printing electrode, and puts into subsequently mercury electrode and platinum electrode and carries out Differential Pulse Voltammetry and detect.Location parameter: initial potential is-0.1V, final current potential 0.7V, sweep velocity is 4mV/s, and pulse height is 50mV, and the sampling time is 20 seconds, and pulse width is 60 milliseconds, and the recurrence interval is 2000 milliseconds, and be 2 seconds rest time.
The in the situation that of each parameter constant, change dopamine concentration and be respectively 1 * 10
-7mol/L, 2.5 * 10
-7mol/L, 5 * 10
-7mol/L, 7.5 * 10
-7mol/L and 10 * 10
-7mol/L reacts.
Fig. 4 is that dopamine concentration is respectively 1 * 10
-7mol/L, 2.5 * 10
-7mol/L, 5 * 10
-7mol/L, 7.5 * 10
-7mol/L, 10 * 10
-7concentration-the map of current being depicted as during mol/L, dopamine concentration is 0.5 * 10
-7mol/L ~ 10 * 10
-7within the scope of mol/L, there is good linear relationship with coupled product oxidation peak current, by Fig. 4, show that linear equation is: lp=0.992 * C
dopamine+ 0.313, coefficient R
2be 0.989, lowest detection is limited to 0.5 * 10
-7mol/L.Linear relationship by Fig. 4 can be drawn by the numerical value of the peak current of magnetic field measuring dopamine after coupling the concentration of dopamine solution to be measured.
Claims (8)
1. the electrolytic cell for detection of dopamine, wherein, comprise that Chi Tiji is positioned over the working electrode of Chi Tizhong, to electrode and contrast electrode, described pond body comprises Chi Gai, at the bottom of solution pool and pond, cover strip hole, described pond, described solution pool is inverted round stage shape, at the bottom of described pond, be cylindrical, at the bottom of described pond, in the middle of bottom, be provided with shrinkage pool, in described shrinkage pool, magnet is housed, described magnet lower end is provided with spring, described working electrode crosses at junction at the bottom of described solution pool and pond, the working portion of described working electrode is towards solution pool, described electrode and contrast electrode are inserted in the hole of Chi Gai, the described working portion to electrode and contrast electrode enters in solution pool.
2. a kind of electrolytic cell for detection of dopamine according to claim 1, wherein, passes through fastened by screw at the bottom of described solution pool and pond, and at the bottom of described solution pool and pond, junction is provided with rubber blanket.
3. a kind of electrolytic cell for detection of dopamine according to claim 2, wherein, adopts teflon material at the bottom of described solution pool, Chi Gai and pond, and the bottom of described electrolytic cell is coated with steel plate.
4. a kind of electrolytic cell for detection of dopamine according to claim 3, wherein, described working electrode is selected printing carbon electrode, and the carbon paste district of described printing carbon electrode is circular, described electrode is selected to platinum electrode, and described contrast electrode is selected mercury electrode.
5. application is according to the method for the detection dopamine of the electrolytic cell described in any one in claim 1-4, comprise: under buffer system, by magnetic microsphere and the dopamine solution generation coupling reaction after activation, coupling reaction product is enriched in working electrode surface under magnetic field that electrolytic cell adds, by Differential Pulse Voltammetry, detect peak current, by peak current and standard specimen concentration, set up linear relationship, by set up linear relationship, draw testing sample concentration.
6. a kind of method that detects dopamine according to claim 5, wherein, described working electrode is selected printing carbon electrode.
7. a kind of method that detects dopamine according to claim 6, wherein, described buffer system is selected acetic acid-sodium-acetate buffer.
8. a kind of method that detects dopamine according to claim 7, wherein, the activator of using in described reactivation process is carbodiimide.
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Cited By (2)
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| CN110308189A (en) * | 2019-06-28 | 2019-10-08 | 湖北科技学院 | A kind of Screen-printed electrochemical biosensor and its application for mercury ion detecting |
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| CN110308189A (en) * | 2019-06-28 | 2019-10-08 | 湖北科技学院 | A kind of Screen-printed electrochemical biosensor and its application for mercury ion detecting |
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