CN1769884A - Capillary electrophoresis chip integrated with electrochemical detection electrode made by hot pressing method - Google Patents
Capillary electrophoresis chip integrated with electrochemical detection electrode made by hot pressing method Download PDFInfo
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- CN1769884A CN1769884A CN 200510010371 CN200510010371A CN1769884A CN 1769884 A CN1769884 A CN 1769884A CN 200510010371 CN200510010371 CN 200510010371 CN 200510010371 A CN200510010371 A CN 200510010371A CN 1769884 A CN1769884 A CN 1769884A
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Abstract
The invention relates to an electrophoresis chip of high polymer substrate capillary tubes which comprises base-plate, cover plate and metal wire detecting electrode. On the base-plate having sampling and separating micro channel, buffer solution pool and sampling pool; the metal wire being embedded on the cover plate by separating or performing as electrochemical detecting electrode; micro channel, buffer solution pool on the base-plate being made by mechanical engraving or casting molding; the base-plate and cover plate being made by heat pressing or being bond by chemical method to form electrophoresis chip. The inventive electrophoresis chip has the advantages of being used for separating and detecting mineral ions, organic molecule, amino acid and proteins.
Description
(1) technical field
What the present invention relates to is a kind of superpolymer Capillary Electrophoresis microchip of suitable Electrochemical Detection, particularly is micromolecular separation such as a kind of suitable micro-inorganic anion, kation, amino acid and the integrated Capillary Electrophoresis microchip of electrochemical detection electrode that detects usefulness.
(2) background technology
Capillary Electrophoresis is a kind of new and effective separation, analytical technology.It is one of research field of analytical chemistry forefront.In recent years, few with its amount of samples based on the Capillary Electrophoresis microchip of MEMS technology, disengaging time is short, is easy to the integrated and microminiaturized of system, and advantages such as suitable mass production develop rapidly, become the frontier of capillary electrophoresis technique high speed development.The Capillary Electrophoresis microchip is silicon chip, the glass several square centimeters of sizes, or adopts photoetching, the corrosion technology of integrated circuit on other high polymer material, and the chip that has microstructures such as raceway groove, liquid pool, electrode of other micro-processing technology making.
Adopt silicon wafer to manufacture Capillary Electrophoresis microchip, can utilize ripe integrated circuit technology and silicon micromachining technology, have the manufacture craft maturation, be easy to integrated and advantage mass production, but the electrical insulating property of silicon chip is poor, separation voltage is low, and there is light transmission poor, shortcomings such as price height.Glass-based Capillary Electrophoresis microchip has advantages such as electrical insulating property is good, light transmission is strong, is the maximum and commercial capillary electrophoresis chip of current research, but the glass-based chip have be difficult to integrated, the encapsulation of glass/glass needs the high temperature bonding, and cost of manufacture is higher, shortcomings such as price height.And superpolymer Capillary Electrophoresis microchip mainly is organic glass material and PDMS material, is generally had an optimistic view of in recent years, is low-cost, and the simple capillary electrophoresis chip of job operation has vast potential for future development.
The detection method of capillary electrophoresis chip mainly contains UV Absorption, laser-induced fluorescence (LIF) and Electrochemical Detection etc.Laser-Induced Fluorescence Detection has very high sensitivity, but because the instrument volume is bigger, is difficult to integratedly, is unfavorable for the microminiaturization of system.It is wide that UV Absorption detects detectable material scope, but sensitivity is low, and light source is big, also is difficult to integrated and microminiaturization system.Electrochemical Detection is a big class analysis test method commonly used.No matter which kind of electrochemical assay all adopts electrode as sensor, directly the chemical signal with component to be measured in the solution changes electric signal into.This sensing mode meets the microminiaturization of capillary electrophoresis analysis system, integrated requirement very much.Because: (1) makes microelectrode by the MEMS technology on chip not difficult, and this is more much easier than processing micro-optical device on chip; (2) different with optical detection, the sensitivity of electrochemical sensing can't reduce because passage gathers the microminiaturization of yardstick; (3) peripherals such as signal processing system of electrochemical detector are fairly simple, and are easily microminiaturized.Therefore as the integrated detection mode of micro-full analytical system, electrochemical detector has special advantages.According to the difference of Electrochemical Detection principle, at present the electrochemical detector that is adopted in detection system at the kapillary electricity mainly contains ampere detector, electric conductivity detector and potential monitoring device.
(3) summary of the invention
The objective of the invention is for a kind of detecting electrode that has long split tunnel to become with chip integration is provided, have higher sensitivity and separation efficiency, interference little, can be used for polycomponent and measure, the capillary electrophoresis chip of integrated electrochemical detecting electrode simple in structure, the present invention also aims to provide that a kind of manufacture craft is easy, with low cost, the capillary electrophoresis chip of the integrated with electrochemical detection electrode made by hot pressing method being convenient to operate.
Purpose of the present invention can realize by following measure:
It comprises substrate and cover plate; On substrate, establish two sample cells, 1,3, two buffer pools 2,4; Wherein two sample cells 1,3 are communicated with by sample intake passage, and two buffer pools 2,4 are connected by split tunnel, and intersect vertically with sample intake passage; Sample cell corresponding with position on the substrate and buffering liquid pool are being arranged on the cover plate, and corresponding connection with position on the substrate, it is characterized in that: inlay the detecting electrode tinsel in the terminal relevant position of split tunnel; Substrate and cover plate are bonded to one.。
The above-mentioned substrate and the material of cover plate are selected from poly-methyl-prop diluted acid formicester (PMMA), the transparent superpolymer of dimethyl silicone polymer (PDMS), polystyrene, Polyvinylchloride, phenolics, resin, polyurethane, poly-several lactams or any multipolymer between them.When superpolymer was organic glass matrix, wire electrode was to be embedded on the cover plate with hot-press method; When superpolymer was PDMS matrix, wire electrode directly was mounted on the cover plate when the cast cover plate.Tinsel can be Ag, Au, Pt, and diameter is at 0.1-0.8mm.
When adopting electricity to lead to detect, test electrode and to separate raceway groove vertical, apart from damping fluid waste liquid pool 1.5-3mm, two test electrodes are the 0.3-1 millimeter apart; When adopting Amperometric Detection Coupled, the ground end of separate mesh electrode is a palladium electrode, decoupling and the effect of row's hydrogen are arranged, palladium electrode is with to separate raceway groove vertical, and apart from damping fluid waste liquid pool 1-3 millimeter, the Amperometric Detection Coupled working electrode is also with to separate raceway groove vertical, separating the raceway groove port, with the tangent position of damping fluid waste liquid pool, the placement requirement of contrast electrode is aimed at the outlet of splitter box road is strict, and electrode position is apart from 2～50 microns of splitter box road outlets.
The present invention has following advantage than prior art:
The present invention combines tinsel electrochemical detection electrode and capillary electrophoresis chip, the kapillary electricity of making is compared with the chip of the electrochemical detection electrode that chip and known employing IC standard technology are made, have simple for process, the yield rate height, advantages such as chip is easy to use, and is with low cost.
(4) description of drawings
Fig. 1 conductance detection PMMA substrate straight channel capillary electrophoresis chip synoptic diagram;
Fig. 2 conductance detection PDMS substrate is bent passage capillary electrophoresis chip synoptic diagram;
Fig. 3 Amperometric Detection Coupled method PDMS substrate is bent passage capillary electrophoresis chip synoptic diagram.
Among the figure: 1-sample cell, 3-sample waste liquid pool, 2-buffer pool, 4-damping fluid waste liquid pool, 5-sample intake passage, 6-split tunnel, 7-silver wire electrode, 8-platinum electrode, 9-palladium silk electrode, 10-Amperometric Detection Coupled contrast electrode, 11-Amperometric Detection Coupled working electrode
(5) embodiment
Fig. 1 is embodiment 1: conductance detection PMMA substrate straight channel capillary electrophoresis chip synoptic diagram.
(1) making of substrate: base material is a polymethylmethacrylate, adopts micromachined mode cunning to carve the chip raceway groove, and concrete grammar is seen patent of invention 03111185.3 " a kind of be used for the capillary electrophoresis chip method for making that chemical analysis is used ".100 microns of sample intake passage and split tunnel width upper bases are gone to the bottom 50 microns, 50 microns of the degree of depth, and long 1 centimetre of sample intake passage, split tunnel length is 5 centimetres.
(2) making of cover plate: with the substrate of the same material of substrate, size on, select and the corresponding position of substrate liquid pool, with miniature bench drill punching, the diameter in hole depends on the diameter of drill bit, when drill bit was 2 millimeters a diamond bit, the diameter in hole was 2 millimeters of liquid pool diameters.Carve detecting electrode position cut in 2 millimeters cunnings of split tunnel end-to-end distance damping fluid waste liquid pool, at a distance of 500 microns, Ag silk electrode is placed the cut place between two electrodes, hot pressing is fixed on hot press, pressure 7.0Kg, 95 ℃ of temperature, 1min takes off, and 100 microns thick 2 Ag silk electrodes are bumped into cover plate.
(3) hot press: substrate and cover plate applying is fixing, and pressurization 7.0Kg is warming up to 100 ℃ of heating 5 minutes, naturally cools to room temperature then, and chip join is firm.
Fig. 2 is embodiment 2: conductance detection PDMS substrate is bent passage capillary electrophoresis chip synoptic diagram.
(1) making of substrate: base material is dimethyl silicone polymer PDMS, and its main technique flow process is: make chip formpiston-join in 1: 1 the ratio bonding of PDMS performed polymer and the hardening agent-casting curing-demoulding-substrate and cover plate.Concrete grammar is seen patent of invention 200510009804.9 " a kind of is the simple and easy irreversible bonding method of chip of base material with the dimethyl silicone polymer ".
(2) making of cover plate: with the substrate of the same size of the same material of substrate on, selected and the corresponding position of substrate liquid pool are with card punch punching, 1 millimeter of liquid pool diameter.2 millimeters places imbed detecting electrode at split tunnel end-to-end distance damping fluid waste liquid pool, between two electrodes at a distance of 500 microns, imbed 2 at 50 microns thick Pt silk electrodes, this group electrode PDMS does not put into during polymerization, treats that polymerization process finishes just firm being inlaid in the PDMS chip of electrode.
(3) bonding of substrate and cover plate: concrete grammar is seen patent of invention 200510009804.9 " a kind of is the simple and easy irreversible bonding method of chip of base material with the dimethyl silicone polymer ".
Fig. 3 is embodiment 3: Amperometric Detection Coupled method PDMS substrate is bent passage capillary electrophoresis chip synoptic diagram.
(1) making of substrate: base material is dimethyl silicone polymer PDMS, and its main technique flow process is: making chip formpiston-join PDMS performed polymer and the hardening agent-casting curing-demoulding-bonding in 1: 1 ratio.Concrete grammar is seen patent of invention 200510009804.9 " a kind of is the simple and easy irreversible bonding method of chip of base material with the dimethyl silicone polymer ".
(2) making of cover plate: with the substrate of the same size of the same material of substrate on, selected and the corresponding position of substrate liquid pool are with card punch punching, 1 millimeter of liquid pool diameter.Imbed electrophoretic separation ground end palladium electrode at 1.5 millimeters places of split tunnel end-to-end distance damping fluid waste liquid pool, palladium electrode is with to separate raceway groove vertical.The Amperometric Detection Coupled working electrode is embedded in the damping fluid waste liquid pool, and the raceway groove port is vertical with separating.
(3) bonding of substrate and cover plate: concrete grammar is seen patent of invention 200510009804.9 " a kind of is the simple and easy irreversible bonding method of chip of base material with the dimethyl silicone polymer ".
Claims (5)
1, a kind of capillary electrophoresis chip of integrated with electrochemical detection electrode made by hot pressing method, it comprises substrate and cover plate; On substrate, establish two sample cells (1), (3), two buffer pools (2), (4); Wherein two sample cells (1), (3) are communicated with by sample intake passage, and two buffer pools (2), (4) are connected by split tunnel, and intersect vertically with sample intake passage; Sample cell corresponding with position on the substrate and buffering liquid pool are being arranged on the cover plate, and corresponding connection with position on the substrate, it is characterized in that: inlay the detecting electrode tinsel in the terminal relevant position of split tunnel; Substrate and cover plate are bonded to one.
2., the capillary electrophoresis chip of integrated with electrochemical detection electrode made by hot pressing method as claimed in claim 1, it is characterized in that: the superpolymer matrix of substrate and patch material is polymethylmethacrylate, with hot-press method wire electrode is embedded on the cover plate, tinsel is Cu, Ag, Au, Pt or Pd, and diameter is at 0.01-0.8mm.
3, the capillary electrophoresis chip of integrated with electrochemical detection electrode made by hot pressing method as claimed in claim 1, it is characterized in that: the superpolymer matrix of substrate and patch material is dimethyl silicone polymer, wire electrode directly is mounted on the cover plate, tinsel is Cu, Ag, Au, Pt or Pd, and diameter is at 0.01-0.8mm.
4, as the capillary electrophoresis chip of claim 1,2 or 3 described integrated with electrochemical detection electrode made by hot pressing method, it is characterized in that: test electrode is with to separate raceway groove vertical, and apart from damping fluid waste liquid pool 0.5-3mm, two test electrodes are at a distance of 0.3-1mm.
5, as the capillary electrophoresis chip of claim 1,2 or 3 described integrated with electrochemical detection electrode made by hot pressing method, it is characterized in that: the ground end of separate mesh electrode is a palladium electrode, palladium electrode is with to separate raceway groove vertical, apart from damping fluid waste liquid pool 1-3 millimeter, the Amperometric Detection Coupled working electrode is separating raceway groove port and the tangent position of damping fluid waste liquid pool also with to separate raceway groove vertical, contrast electrode is aimed at the outlet of splitter box road, and electrode position is apart from 2～50 microns of splitter box road outlets.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101622532A (en) * | 2007-04-27 | 2010-01-06 | 爱科来株式会社 | Analysis chip and analysis apparatus |
| CN102253102A (en) * | 2011-04-07 | 2011-11-23 | 重庆大学 | Micro-fluidic composite chip with symmetric micro-channel structure and integrated non-contact conductivity detection |
| CN106093168A (en) * | 2016-06-14 | 2016-11-09 | 中国科学院合肥物质科学研究院 | Phosphate radical electrochemical sensor based on MEMS technology and the application in dynamically detection phosphate radical thereof |
| CN106596692A (en) * | 2017-01-14 | 2017-04-26 | 常州大学 | Method for detecting interaction of antibody and polypeptide through tortuous capillary electrophoresis |
| CN113758988A (en) * | 2020-05-18 | 2021-12-07 | 昆山聂尔精密仪器有限公司 | Device and method for controlling enrichment and separation of liquid-phase ions and multi-electrode chip |
-
2005
- 2005-09-28 CN CN 200510010371 patent/CN1769884A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487491B (en) * | 2007-04-27 | 2015-09-02 | 爱科来株式会社 | Analysis chip and analytical equipment |
| CN103487490B (en) * | 2007-04-27 | 2015-10-28 | 爱科来株式会社 | Analysis chip and analytical equipment |
| CN101622532B (en) * | 2007-04-27 | 2013-08-14 | 爱科来株式会社 | Analysis chip and analysis apparatus |
| CN101622532A (en) * | 2007-04-27 | 2010-01-06 | 爱科来株式会社 | Analysis chip and analysis apparatus |
| CN103487491A (en) * | 2007-04-27 | 2014-01-01 | 爱科来株式会社 | Analysis chip and analysis apparatus |
| CN103487490A (en) * | 2007-04-27 | 2014-01-01 | 爱科来株式会社 | Analysis chip and analysis apparatus |
| CN102253102B (en) * | 2011-04-07 | 2013-10-30 | 重庆大学 | Micro-fluidic composite chip with symmetric micro-channel structure and integrated non-contact conductivity detection |
| CN102253102A (en) * | 2011-04-07 | 2011-11-23 | 重庆大学 | Micro-fluidic composite chip with symmetric micro-channel structure and integrated non-contact conductivity detection |
| CN106093168A (en) * | 2016-06-14 | 2016-11-09 | 中国科学院合肥物质科学研究院 | Phosphate radical electrochemical sensor based on MEMS technology and the application in dynamically detection phosphate radical thereof |
| CN106093168B (en) * | 2016-06-14 | 2018-12-07 | 中国科学院合肥物质科学研究院 | Phosphate radical electrochemical sensor based on MEMS technology and its application in dynamic detection phosphate radical |
| CN106596692A (en) * | 2017-01-14 | 2017-04-26 | 常州大学 | Method for detecting interaction of antibody and polypeptide through tortuous capillary electrophoresis |
| CN106596692B (en) * | 2017-01-14 | 2018-12-28 | 常州大学 | A kind of method of tortuous capillary electrophoresis detection antibody polypeptides interaction |
| CN113758988A (en) * | 2020-05-18 | 2021-12-07 | 昆山聂尔精密仪器有限公司 | Device and method for controlling enrichment and separation of liquid-phase ions and multi-electrode chip |
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