CN1379240A - Capillary tube electrophoresis-solid electrochemical luminescence detector and its preparing process - Google Patents
Capillary tube electrophoresis-solid electrochemical luminescence detector and its preparing process Download PDFInfo
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- CN1379240A CN1379240A CN 02116453 CN02116453A CN1379240A CN 1379240 A CN1379240 A CN 1379240A CN 02116453 CN02116453 CN 02116453 CN 02116453 A CN02116453 A CN 02116453A CN 1379240 A CN1379240 A CN 1379240A
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- capillary tube
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Abstract
An electrochemical luminou s solid detector for capillary tube electrophoresis features that the sulfonic acid polymer A, sol-gel, and polyvinyl alcohol graft copolymer are mixed to obtain a high-molecular mixture rich in sulfonic acid groups, which is used to adsorb triple pyridineruthenium. The membrane material is fixed on the surface of microelectrode by rotary coating to obtain the said detector.
Description
Technical field: the invention belongs to capillary tube electrophoresis-solid electrochemical luminescence detector and preparation method.
Background technology: the electrochemiluminescence detection technique (ECL) of tris (bipyridine) ruthenium is one of method the sensitiveest in the electrochemical measuring technique, is used for the detection of drug molecule, amino acid, polypeptide, protein and nucleic acid.The luminous detecting pattern of common Capillary Zone Electrophoresis with Electrochemical is the cathode pool that the terpyridyl ruthenium solution is placed Capillary Electrophoresis, the amount of expending of reagent is bigger like this, because tris (bipyridine) ruthenium reagent is comparatively expensive, therefore this pattern and be not suitable for promoting the use of widely.
Summary of the invention: the material that the purpose of this invention is to provide a kind of capillary tube electrophoresis-solid electrochemical luminescence detector;
Another object of the present invention provides a kind of preparation method of capillary tube electrophoresis-solid electrochemical luminescence detector.
The present invention adopts sulfonic acid polymer and sol-gel and polyvinyl alcohol graft copolymerized copolymer blended first, and tris (bipyridine) ruthenium is fixed on the surface of microelectrode, the preparation capillary tube electrophoresis-solid electrochemical luminescence detector.The reagent consumption of tris (bipyridine) ruthenium lacking very.
The present invention adopts polystyrolsulfon acid and sol-gel and polyvinyl alcohol graft copolymerized copolymer blended, forms and is rich in the polymer blended material of sulfonic acid group, and tris (bipyridine) ruthenium is adsorbed in this material.The purpose that adopts sol-gel is to make membrane material form three-dimensional structure.Adopt the purpose of polyvinyl alcohol graft copolymerized multipolymer to be the structural stability of reinforcing membrane.Membrane material is fixed on the surface of microelectrode through spin coating, forms solid electrochemical luminescence detector.
The mass ratio of polystyrolsulfon acid, sol-gel and polyvinyl alcohol graft copolymerized multipolymer is 1: 1～100: 1～100, and the concentration of tris (bipyridine) ruthenium is in 0.2 polystyrolsulfon acid 10mM scope, and electrode material can be a metal electrode, as gold, and platinum; Also can carbon-based electrode, as glass-carbon electrode, graphite electrode.
Preparation process: get 1% polystyrolsulfon acid solution, 10 μ L, add the sol-gel solution of 10～100 μ L 16.8%, the 20% graft copolymer solution of 8～80 μ L, and the ultrasonic blend of 20mM tris (bipyridine) ruthenium of 1～200 μ L; Get 1 μ L and be added drop-wise to the surface of microelectrode, after 3000～8000 rev/mins speed is coated with 30～120 seconds, electrode was positioned in the refrigerator 1～12 hour, prepare the capillary tube electrophoresis-solid electrochemical luminescence detector that tris (bipyridine) ruthenium is modified, during use this detecting device is placed on the exit of capillary end.
Embodiment is as follows:
Embodiment 1: get 1% polystyrolsulfon acid solution, 10 μ L, add the sol-gel solution of 10 μ L 16.8%, the 20% graft copolymer solution of 8 μ L, and the ultrasonic blend of 20mM tris (bipyridine) ruthenium of 1 μ L.Get 1 μ L and be added drop-wise to the surface of microelectrode, after 3000 rev/mins speed is coated with 30 seconds, electrode was positioned in the refrigerator 1 hour, prepared the capillary tube electrophoresis-solid electrochemical luminescence detector that tris (bipyridine) ruthenium is modified, and during use this detecting device was placed on the exit of capillary end.
The detection of tripropyl amine (TPA) and proline
Electrode is put into the Capillary Electrophoresis cathode pool of the phosphate solution pH=9.5 that contains 0.1M, and electrode is placed on exit capillaceous, and internal diameter capillaceous is 75 μ m.To the detection of tripropyl amine (TPA) and proline as shown in Figure 1, Capillary Electrophoresis-electrochemistry of solids luminescence detector is measured TPA (1) and proline, separation voltage 15KV; Electronic sampling, 15KV3 second; Detect current potential 1.1V; Electrophoretic buffer 10mM phosphate.This shows that this electrode pair detection of amines has good sensitivity.
Embodiment 2: get 1% polystyrolsulfon acid solution, 10 μ L, add the sol-gel solution of 50 μ L 16.8%, the 20% graft copolymer solution of 20 μ L, and the ultrasonic blend of 20mM tris (bipyridine) ruthenium of 50 μ L.Get 1 μ L and be added drop-wise to the surface of microelectrode, after 6000 rev/mins speed is coated with 1 minute, electrode was positioned in the refrigerator 6 hours, prepared the capillary tube electrophoresis-solid electrochemical luminescence detector that tris (bipyridine) ruthenium is modified, and during use this detecting device was placed on the exit of capillary end.
The detection of tripropyl amine (TPA) (TPA)
Electrode is put into the Capillary Electrophoresis cathode pool of the phosphate solution pH=7.5 that contains 0.1M, and electrode is placed on exit capillaceous, and internal diameter capillaceous is 75 μ m.Standard deviation to the continuous six times detection of tripropyl amine (TPA) is 9.8%.Electrode soaked in the phosphate of 0.1M after 16 hours, and the sensitivity of detecting device does not significantly descend.This shows that this detecting device detects TPA has good stability.
Embodiment 3: get 1% polystyrolsulfon acid solution, 10 μ L, add the sol-gel solution of 100 μ L 16.8%, the 20% graft copolymer solution of 80 μ L, and the ultrasonic blend of 20mM tris (bipyridine) ruthenium of 200 μ L.Get 1 μ L and be added drop-wise to the surface of microelectrode, after 8000 rev/mins speed is coated with 2 minutes, electrode was positioned in the refrigerator 12 hours, prepared the capillary tube electrophoresis-solid electrochemical luminescence detector that tris (bipyridine) ruthenium is modified, and during use this detecting device was placed on the exit of capillary end.
The mensuration of oxalate denominationby:
Electrode is put into the Capillary Electrophoresis cathode pool of the metabisulfite solution pH=7.0 that contains 0.1M, and electrode is placed on exit capillaceous, and internal diameter capillaceous is 50 μ m.Standard deviation to the continuous six times detection of oxalate denominationby is 6.5%, and the sensitivity of detection is 0.1 μ mol/L.This shows that this detecting device detects oxalate has higher sensitivity.
Claims (3)
1. the material of a capillary tube electrophoresis-solid electrochemical luminescence detector, form by polystyrolsulfon acid, sol-gel and polyvinyl alcohol graft copolymerized multipolymer, its mass ratio is 1: 1～100: 1～100, the concentration of tris (bipyridine) ruthenium is in 0.2 polystyrolsulfon acid 10mM scope, electrode material can be metal electrode gold, platinum; Also can be carbon-based electrode: glass-carbon electrode, graphite electrode.
2. the preparation method of a capillary tube electrophoresis-solid electrochemical luminescence detector, it is characterized in that getting 1% polystyrolsulfon acid solution, 10 μ L, the sol-gel solution that adds 10～100 μ L 16.8%, the 20% graft copolymer solution of 8～80 μ L, and the ultrasonic blend of 20mM tris (bipyridine) ruthenium of 1～200 μ L; Get 1 μ L and be added drop-wise to the surface of microelectrode, after 3000～8000 rev/mins speed was coated with 30～120 seconds, electrode was positioned in the refrigerator 1～12 hour, made the capillary tube electrophoresis-solid electrochemical luminescence detector that tris (bipyridine) ruthenium is modified.
3. the preparation method of capillary tube electrophoresis-solid electrochemical luminescence detector as claimed in claim 2 is characterized in that comprising the material mixture ratio that uses claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02116453 CN1379240A (en) | 2002-04-05 | 2002-04-05 | Capillary tube electrophoresis-solid electrochemical luminescence detector and its preparing process |
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| CN 02116453 CN1379240A (en) | 2002-04-05 | 2002-04-05 | Capillary tube electrophoresis-solid electrochemical luminescence detector and its preparing process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1314622C (en) * | 2005-04-30 | 2007-05-09 | 中国科学院长春应用化学研究所 | Process for preparing electrochemistry luminous sensor of Nafion carbon ceramic composite material |
| CN100392387C (en) * | 2005-09-23 | 2008-06-04 | 中国科学院长春应用化学研究所 | A method for immobilizing ruthenium terpyridine on the surface of an electrochemical electrode |
| CN1882839B (en) * | 2003-09-24 | 2011-08-10 | 原子能委员会 | Devices for the separation and/or analysis of different molecular targets in complex mixtures |
-
2002
- 2002-04-05 CN CN 02116453 patent/CN1379240A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1882839B (en) * | 2003-09-24 | 2011-08-10 | 原子能委员会 | Devices for the separation and/or analysis of different molecular targets in complex mixtures |
| CN1314622C (en) * | 2005-04-30 | 2007-05-09 | 中国科学院长春应用化学研究所 | Process for preparing electrochemistry luminous sensor of Nafion carbon ceramic composite material |
| CN100392387C (en) * | 2005-09-23 | 2008-06-04 | 中国科学院长春应用化学研究所 | A method for immobilizing ruthenium terpyridine on the surface of an electrochemical electrode |
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