CN104568927A - Electrochemical luminescence device and method - Google Patents
Electrochemical luminescence device and method Download PDFInfo
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- CN104568927A CN104568927A CN201510030949.0A CN201510030949A CN104568927A CN 104568927 A CN104568927 A CN 104568927A CN 201510030949 A CN201510030949 A CN 201510030949A CN 104568927 A CN104568927 A CN 104568927A
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Abstract
The invention discloses an electrochemical luminescence device and an electrochemical luminescence method. The electrochemical luminescence device comprises a photomultiplier, a special convex system and an electrochemical luminescence battery containing an electrochemical luminescence analysis solution, wherein a divergent light signal emitted by an electrochemical luminescence battery in the past is collected and focused on the photomultiplier through the convex lens system, so that the intensity of the detected light signal can be greatly enhanced; and the sensitivity of an electrochemical luminescence instrument and an analysis method is improved. A to-be-detected solution is put into the electrochemical luminescence battery, and corresponding electrochemical scanning determination is carried out. An electrochemical luminescence signal which is diverged in advance is focused on the photomultiplier under the condition of invariable quantum dot variety, so that accurate measurement of low-concentration components is achieved. An electrochemical luminescence focusing device meets the condition: 1/object distance+1/image distance=1/lens focus distance by the convex lens imaging principle; and the detection sensitivity of the electrochemical luminescence method can be greatly improved under the condition that an electrochemical reaction system is not changed.
Description
Technical field
The present invention relates to electrochemical techniques, in particular, relate to a kind of electrochemiluminescence device and method.
Background technology
Electrogenerated chemiluminescence (ECL) is the product that galvanochemistry and chemiluminescence combine.It refers to the electron transfer reaction generation excited state by electrode surface, produces the phenomenon of optical radiation when it returns ground state.ECL experiences two processes: electrochemical reaction and chemiluminescence reaction.Relative to Photoluminescence Analysis, ECL is that electricity starts, and without the need to excitation source, effectively prevent parasitic light and impure the produced interference of light source, greatly adds the sensitivity of analysis.
On the other hand, as carrier important in electrogenerated chemiluminescence technology, semiconductor nanocrystal, i.e. quantum dot, have unique photoelectric property, be widely used in light emitting diode, photoelectric conversion material, fluorescence probe and bio-imaging field.It is as a kind of emerging ECL luminophor, and quantum dot ECL analyzes to become in Electroanalytical Chemistry field a very active study hotspot, has played vital role in the building process of ECL bio-sensing strategy.
The quantum dot that at present existing all size, pattern are different is used as the luminophor of ECL, for bioanalysis detection field, provides a good platform for building new E CL biology sensor.However, with traditional ECL system (Ru (bpy)
3 2+/ tripropyl amine (TPA)) compare, still there is many weak points in the ECL of quantum dot.Quantum dot ECL intensity is weak, and the existence of the problems such as ECL spectral width, seriously constrains its further developing in field of bioanalysis.
Electrochemial luminescence detecting instrument is surveying instrument important in electroluminescent technology, has simple to operate, sensitivity and accuracy high, good selective.But due to when quantum dot concentration is certain, luminous intensity cannot continue to increase; In addition, in electrochemiluminescence instrument used at present, there is no optical focusing system, at the photon that electrode surface produces, propagate to surrounding, only seldom a part can arrive on the detection auroral poles of photomultiplier, fails to make full use of the luminous signal that electrochemical reaction produces, greatly limit the further raising of detection sensitivity, be unfavorable for the mensuration of trace components.
Summary of the invention
In view of this, the invention provides a kind of electrochemiluminescence device and method, to improve the detection sensitivity of existing electrochemiluminescence instrument and method further.
For achieving the above object, the invention provides following technical scheme:
A kind of electrochemiluminescence device, the convex lens group of particular focal length is housed in the photomultiplier transit tube cassette of Electrochemial luminescence detecting instrument, it is made to meet the image-forming condition of 1/u (object distance)+1/v (image distance)=1/f (focal length of lens), the light signal sent by electrode surface converges and is imaged on the responsive auroral poles of photomultiplier, to remain unchanged and under identical testing conditions at original device, increase substantially the sensitivity of instrument, realize the Measurement accuracy to trace components.
To achieve these goals, the present invention adopts following technical scheme:
A kind of electrochemiluminescence device, comprises photomultiplier, convex lens system and electrochemiluminescence pond; Wherein, convex systems is arranged between electrochemiluminescence pond and photomultiplier, forms straight line; The light that electrochemiluminescence pond sends all is focused on the photoactive electrode of photomultiplier by convex systems; The focal length of convex systems meets convex lens condition: 1/ object distance+1/ image distance=1/ focal length of lens, electrochemiluminescence is provided with three-electrode system in pond, working electrode height adjustable, to obtain best spotlight effect.
Described three-electrode system, electrochemiluminescence pond, convex lens system and photomultiplier are all arranged in magazine, corresponding to wire connection electroluminescence detector in magazine, electroluminescence detector connects electroluminescence analyser, and electroluminescence analyser connects computing machine and carries out optimum configurations and data acquisition.
Described convex lens system comprises about two convex lens distributed, and the convex lens position being wherein placed in upper end is adjustable.
Described convex lens material is quartz, glass or plastics.
Described three-electrode system, comprises working electrode, contrast electrode and to electrode, is all placed in electrochemiluminescence pond, the electrochemiluminescence analysis solution in contact electrochemiluminescence pond.
Preferably, described working electrode is glass-carbon electrode, gold electrode, and contrast electrode is Ag-AgCl electrode, saturated calomel electrode, is platinum electrode to electrode.
Preferably, the diameter of described glass-carbon electrode is 5.0mm.
The voltage of described photomultiplier is set to 400V ~ 600V, and luminous progression is 1 ~ 3 grade.
Described magazine is metal shell.
Based on a using method for said apparatus, comprise the following steps:
(1) connect whole device, carry out instrument preheating;
(2) clean electrochemiluminescence pond, the quantum dot of set amount, coreagent, buffer solution and determinand are mixed, leave standstill, put into electrochemiluminescence pond;
(3) three-electrode system is put into the electrochemiluminescence pond filling liquid to be measured, put into magazine, be connected with the wire in magazine, close magazine;
(4) set electrochemical parameter, Photomultiplier tube voltage and luminous progression, measure;
(5) inventory analysis data, cleaning electrode and electrochemiluminescence pond.
The concrete grammar of described step (2) is: cleaned up in electrochemiluminescence pond with the ultrapure water of 18.25M Ω; Before mensuration test substance content, all solution all needs with ultrapure water now with the current; The mixed solution prepared passes into nitrogen deoxygenation again; Magazine is put in electrochemiluminescence pond, and each position measured all should be consistent.
In described step (2), quantum dot, coreagent, buffer solution, suitably, described quantum dot is CdSe, CdTe or CdS to its volume ratio, and concentration is finally at below 0.71umol/L; Described damping fluid comprises PBS buffer solution, Tris buffer solution, carbonate buffer solution; Described coreagent comprises ammonium persulfate, hydrogen peroxide or oxalic acid; The concentration of final constant volume damping fluid and coreagent is 0.1mol/L.
In described step (3), glass-carbon electrode uses 1.0 first successively, the α-Al of 0.3 μm
2o
3burnishing powder polishing, then rinse successively with absolute ethyl alcohol, ultrapure water, nitrogen dries up; Wires cross is prevented, wrong electrode in wiring process; Three-electrode system puts into electrochemiluminescence pond, keeps three electrode lower ends in solution in the same horizontal line, to be closed by magazine, wait to be determined.
In described step (4), select cyclic voltammetry, galvanochemistry and ECL test condition.
In described step (4), when measuring ascorbic acid content: electromotive force window is 0 ~-1.6V, direction of scanning is negative, sweep speed for 50mV/s, solution leads to nitrogen 15-20min, leaves standstill 25 ~ 35s and tests, keep nitrogen atmosphere during test, photomultiplier is high is pressed on 600V, and number of stages of amplification is 1; By electrochemical workstation, ECL signal is produced to the linear ramp that liquid to be measured applies 0 ~-1.6V, collect light signal to photomultiplier with optical focusing system.
Be noted that the detection to different material, the setting of condition is different.
In described step (5), each mensuration is complete, all electrode, electrochemiluminescence pond ultrapure water will be cleaned up, to measure next time.
Principle of work of the present invention is: by the convex lens of the special focal length of installation, the divergent light source that electrochemiluminescence pond sends can be fully focussed on the photosensitive area of photomultiplier, thus improves signal intensity; Two convex lens meet basic image-forming principle and 1/u (object distance)+1/v (image distance)=1/f (focal length of lens); During mensuration, because determinand has quencher or humidification to quantum dot, the luminous intensity of quantum dot will change along with testing concentration change thereupon thus, while noise is constant, signal is exaggerated several times, improves signal to noise ratio (S/N ratio) greatly, improve sensitivity, reduce Monitoring lower-cut, make experimental result more accurate, reliably.
A kind of beneficial effect of electrochemiluminescence Apparatus and system is:
(1) on the basis not changing existing operating conditions, improve the light signal strength that can arrive the responsive auroral poles of photomultiplier, improve the signal to noise ratio (S/N ratio) of detection system, improve the detection sensitivity of ElectrochemiluminescDetermination Determination trace components;
(2) be conducive to reducing error, improve degree of accuracy;
(3) when measuring determinand content, because determinand has quencher or humidification to quantum dot, the luminous intensity of quantum dot will change along with testing concentration change thereupon thus, while noise is constant, signal is exaggerated several times, improve signal to noise ratio (S/N ratio) greatly, improve sensitivity, reduce Monitoring lower-cut.
Accompanying drawing explanation
Fig. 1 is the structural representation of electrochemiluminescence Apparatus and system.
Wherein: 1, magazine; 2, three-electrode system; 3, convex lens system; 4, photomultiplier; 5, computing machine; 6, electroluminescence analytic system electrochemical analyser; 7, electroluminescence analytic system multifunctional chemical luminometer; 8, electrochemiluminescence pond; 9, liquid to be measured.
Embodiment:
Below in conjunction with accompanying drawing and embodiment, electrochemiluminescence Apparatus and system is described further.
As shown in Figure 1, a kind of electrochemiluminescence Apparatus and system, comprise magazine 1, convex systems 3, photomultiplier 4, electroluminescence analytic system electrochemical analyser 6, electroluminescence analytic system multifunctional chemical luminometer 7, wherein three-electrode system 2 is connected with the wire in magazine 1, and electroluminescence analytic system electrochemical analyser 6 is connected with computing machine 5 with electroluminescence analytic system multifunctional chemical luminometer 7.Three-electrode system 2 puts into the electrochemiluminescence pond 8 of being equipped with and detecting liquid 9, closes magazine 1, and computing machine 5 control system is run and detected.
Photomultiplier 4 is photo-detectors that a kind of novel super-high is sensitive, have highly sensitive, dark current is little, signal to noise ratio (S/N ratio) is large, the advantages such as fast response time.In astronomy, nuclear physics, laser, medical treatment ... all be widely used etc. many fields, the use equally in spectrometric instrument is also very general.In ultraviolet-visible spectral limit, nearly all pinpoint spectroscopic analysis instrument all adopts photomultiplier to detect faint light signal, and the quality of the quality of photomultiplier and duty thereof determines the performance of whole instrument to a certain extent.
Magazine 1, convex lens system 3 and photomultiplier 4 are connected to form an entirety, are placed in metal magazine.
Detect the main solution to be measured containing quantum dot, coreagent, damping fluid and each concentration in liquid 9.
Electroluminescence analytic system electrochemical analyser 6 and electroluminescence analytic system multifunctional chemical luminometer 7 are detected by computing machine 5 gauge tap.
Assay method comprises the steps:
1) first according to magazine channel sized design convex systems, the condition of 1/u (object distance)+1/v (image distance)=1/f (focal length of lens) is met.This device comprises: the convex lens that two focal lengths are identical or not identical.One of them lens is fixed on the position in long cylinder darkroom on photomultiplier, makes ECL signal focus at the photosensitive region of photomultiplier; Other convex lens are fixed on the position under magazine on lens, and its position is adjustable.
2) conventionally process cleaning is carried out to electrochemiluminescence pond, electrode, for subsequent use.
3) before measuring, preheating opened by instrument, and in adjustment, convex lens are a suitable position.
4) preparation detects liquid: damping fluid, coreagent and quantum dot are mixed, its volume ratio suitably.Add testing sample, constant volume is to 5mL.
5) three electrodes are put into liquid to be measured, connect wire, close magazine.
6) set instrument parameter, start to measure.
7) in whole observation process, all controlled by computer program, do not need artificial interference, convenient and swift.
8) each measure complete after, timely clearing electrode and electrochemiluminescence pond, clean repeatedly repeatedly.
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 (10)
1. an electrochemiluminescence device, is characterized in that: comprise photomultiplier, convex lens system and electrochemiluminescence pond; Wherein, convex systems is arranged between electrochemiluminescence pond and photomultiplier, forms straight line; The light that electrochemiluminescence pond sends all is focused on the photoactive electrode of photomultiplier by convex systems; The focal length of convex systems meets convex lens condition: 1/ object distance+1/ image distance=1/ focal length of lens, electrochemiluminescence is provided with three-electrode system in pond, working electrode height adjustable.
2. a kind of electrochemiluminescence device as claimed in claim 1, it is characterized in that: described three-electrode system, electrochemiluminescence pond, convex lens system and photomultiplier are all arranged in magazine, corresponding to wire connection electroluminescence detector in magazine, electroluminescence detector connects electroluminescence analyser, and electroluminescence analyser is connected with computing machine and carries out optimum configurations and data acquisition.
3. a kind of electrochemiluminescence device as claimed in claim 1, it is characterized in that: described convex lens system comprises about two convex lens distributed, the convex lens position being wherein placed in upper end is adjustable.
4. a kind of electrochemiluminescence device as claimed in claim 2, is characterized in that: described three-electrode system, comprises working electrode, contrast electrode and to electrode, is all placed in electrochemiluminescence pond, the electrochemiluminescence analysis solution in contact electrochemiluminescence pond.
5. a kind of electrochemiluminescence device as claimed in claim 4, it is characterized in that: described working electrode is glass-carbon electrode, gold electrode, contrast electrode is Ag-AgCl electrode, saturated calomel electrode, is platinum electrode to electrode.
6. based on a using method for the device such as according to any one of claim 1-5, it is characterized in that: comprise the following steps:
(1) connect whole device, carry out instrument preheating;
(2) clean electrochemiluminescence pond, the quantum dot of set amount, coreagent, buffer solution and determinand are mixed, leave standstill, put into electrochemiluminescence pond;
(3) three-electrode system is put into the electrochemiluminescence pond filling liquid to be measured, put into magazine, be connected with the wire in magazine, close magazine;
(4) set electrochemical parameter, Photomultiplier tube voltage and luminous progression, measure;
(5) inventory analysis data, cleaning electrode and electrochemiluminescence pond.
7. using method as claimed in claim 6, is characterized in that: the concrete grammar of described step (2) is: cleaned up in electrochemiluminescence pond with the ultrapure water of 18.25M Ω; Before mensuration test substance content, all solution all needs with ultrapure water now with the current; The mixed solution prepared passes into nitrogen deoxygenation again; Magazine is put in electrochemiluminescence pond, and each position measured all should be consistent.
8. using method as claimed in claim 6, it is characterized in that: in described step (2), quantum dot, coreagent, buffer solution, described quantum dot is CdSe, CdTe or CdS, and concentration is finally at below 0.71umol/L; Described damping fluid comprises PBS buffer solution, Tris buffer solution, carbonate buffer solution; Described coreagent comprises ammonium persulfate, hydrogen peroxide or oxalic acid; The concentration of final constant volume damping fluid and coreagent is 0.1mol/L.
9. using method as claimed in claim 6, is characterized in that: in described step (3), glass-carbon electrode uses 1.0 first successively, the α-Al of 0.3 μm
2o
3burnishing powder polishing, then rinse successively with absolute ethyl alcohol, ultrapure water, nitrogen dries up; Wires cross is prevented, wrong electrode in wiring process; Three-electrode system puts into electrochemiluminescence pond, keeps three electrode lower ends in solution in the same horizontal line, to be closed by magazine, wait to be determined.
10. using method as claimed in claim 6, is characterized in that: in described step (4), selects cyclic voltammetry, galvanochemistry and ECL test condition;
In described step (4), when measuring ascorbic acid content: electromotive force window is 0 ~-1.6V, direction of scanning is negative, sweep speed for 50mV/s, solution leads to nitrogen 15-20min, leaves standstill 25 ~ 35s and tests, keep nitrogen atmosphere during test, photomultiplier is high is pressed on 600V, and number of stages of amplification is 1; By electrochemical workstation, ECL signal is produced to the linear ramp that liquid to be measured applies 0 ~-1.6V, collect light signal to photomultiplier with optical focusing system.
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Cited By (8)
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| CN105717100A (en) * | 2016-04-12 | 2016-06-29 | 山东大学 | Detecting system capable of accurately acquiring ECL (electrochemiluminescence) spectral information |
| CN105842233A (en) * | 2016-05-10 | 2016-08-10 | 山东大学 | Detection system for collecting dual-wavelength electrochemiluminescence light intensity information |
| CN106124753A (en) * | 2016-07-08 | 2016-11-16 | 广州东林生物科技有限公司 | Electrochemiluminescence buffer and cleanout fluid |
| CN107917905A (en) * | 2017-12-29 | 2018-04-17 | 山东师范大学 | Ratio-type photometric analysis device and its detection method based on intelligent terminal |
| CN109030468A (en) * | 2018-08-14 | 2018-12-18 | 四川理工学院 | A kind of electricity enhancing liquid phase chemiluminescence detecting and detection method |
| CN110455886A (en) * | 2019-09-20 | 2019-11-15 | 常熟理工学院 | A kind of photoelectricity COD fast detector |
| CN111028642A (en) * | 2019-12-19 | 2020-04-17 | 方凌花 | Teaching mould for electrochemiluminescence effect |
| CN111157769A (en) * | 2020-01-06 | 2020-05-15 | 广州大学 | Electrochemiluminescence imaging system and imaging method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN105842233A (en) * | 2016-05-10 | 2016-08-10 | 山东大学 | Detection system for collecting dual-wavelength electrochemiluminescence light intensity information |
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| CN107917905A (en) * | 2017-12-29 | 2018-04-17 | 山东师范大学 | Ratio-type photometric analysis device and its detection method based on intelligent terminal |
| CN109030468A (en) * | 2018-08-14 | 2018-12-18 | 四川理工学院 | A kind of electricity enhancing liquid phase chemiluminescence detecting and detection method |
| CN109030468B (en) * | 2018-08-14 | 2024-03-22 | 四川理工学院 | Electric enhancement gas-liquid phase chemiluminescence detection device and detection method |
| CN110455886A (en) * | 2019-09-20 | 2019-11-15 | 常熟理工学院 | A kind of photoelectricity COD fast detector |
| CN111028642A (en) * | 2019-12-19 | 2020-04-17 | 方凌花 | Teaching mould for electrochemiluminescence effect |
| CN111157769A (en) * | 2020-01-06 | 2020-05-15 | 广州大学 | Electrochemiluminescence imaging system and imaging method thereof |
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