CN1804610A - Method and apparatus for capillary electrophoresis direct detection of substance in water-immiscible solution - Google Patents
Method and apparatus for capillary electrophoresis direct detection of substance in water-immiscible solution Download PDFInfo
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- CN1804610A CN1804610A CN 200610018169 CN200610018169A CN1804610A CN 1804610 A CN1804610 A CN 1804610A CN 200610018169 CN200610018169 CN 200610018169 CN 200610018169 A CN200610018169 A CN 200610018169A CN 1804610 A CN1804610 A CN 1804610A
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Abstract
The invention relates to a method and apparatus for using capillary electrophoresis to directly test the material of water-immiscible liquid. The apparatus is mainly formed by a sample pipe and a capillary electrophoresis system. The method adopts a section of water column to seal the water-immiscible solution in the sample pipe, adds sampling voltage, so that the sample extracted to the water column enters into the capillary column buffer solution and the tested material of the immiscible solution transfers to the water column to achieve online back extraction and field sampling to finish the directly test the material of water-immiscible liquid.
Description
Technical Field
The invention relates to a method for directly detecting substances in a water-immiscible solution by using capillary electrophoresis and a device used by the method, belonging to the field of analytical chemistry. The method is characterized by solving the problem of direct detection of capillary electrophoresis of substances in water-immiscible solutions, can be conveniently combined with liquid-liquid extraction, liquid-phase microextraction and other technologies to determine substances in complex biological matrixes and environmental water samples, and has the advantages of simplicity, convenience, rapidness and sensitivity.
Background
Capillary electrophoresis has the characteristics of high sensitivity, high resolution, rapidness, small sample consumption and low cost, and is increasingly widely applied to the fields of environment, biology, medicines, foods and the like in recent years. These sample matrices are often complex and require pretreatment for analysis. Liquid-liquid extraction, liquid-phase microextraction and the like are common sample pretreatment methods. However, the extracts of liquid-liquid extraction and liquid-phase microextraction are not soluble in water, and are not suitable for direct sample injection analysis by capillary electrophoresis. The solvent is usually evaporated and then re-dissolved with a suitable solvent for injection. However, these procedures are time consuming and cumbersome, and furthermore, the analytical reproducibility is poor due to sample evaporation and adsorption on the tube walls.
Disclosure of Invention
In order to overcome the defects caused by solvent volatilization operation, realize the direct sample injection analysis of capillary electrophoresis of an object to be detected in a solution and improve the sensitivity of the method, the invention provides a method for directly detecting substances in a solution immisciblewith water by using capillary electrophoresis and a device used by the method.
The technical scheme adopted by the invention is as follows: firstly, sealing a water immiscible solution in a sample tube by a section of water column (comparing randomly), after the solution and the water column are completely layered in the sample tube, placing the sample tube in a capillary electrophoresis sample introduction position of a capillary electrophoresis system, ensuring that a sample introduction port of a capillary is positioned in the water column, applying sample introduction voltage, enabling a sample extracted into the water column to enter a buffer solution in a capillary column, continuously transferring a substance to be detected in the water immiscible solution into the water column, finally realizing online back extraction and field amplification sample introduction at the same time, and completing the capillary electrophoresis direct detection of the substance in the water immiscible solution.
The invention also provides an on-line back extraction-field amplification sample injection device used by the detection method, which mainly comprises a sample tube and a capillary electrophoresis system, wherein the sample tube is communicated with a buffer solution bottle in the capillary electrophoresis system through a capillary, a water column is used for encapsulating a water-immiscible solution in the sample tube, a separation capillary tube opening of the capillary electrophoresis system is positioned in the water column, and an anode and a cathode are respectively inserted into the water column of the sample tube and the buffer solution in the buffer solution bottle.
After sample introduction voltage is applied, the sample extracted into the water column enters a buffer solution in the capillary column, and the substance to be detected in the water immiscible solution is continuously transferred into the water column, so that the direct separation and detection of the substance in the water immiscible solution by capillary electrophoresis is realized. The method can be used together with liquid-liquid extraction, liquid-phase microextraction and the like, is used for measuring substances in complex biological matrixes and environmental water samples, and has the advantages of simplicity, convenience, rapidness and sensitivity.
The method has the following action principle:
the distribution of the analyte in the organic phase and the water column can be expressed as:
i is the analyte, o represents the organic phase and aq represents the water column.
When a sample is extracted into a water column, some protonation occurs, which can be expressed as:
in electrokinetic sample injection, a field strength hundreds of times higher than that of the electric field in conventional electrophoresis is generated in the water column, and the electric field enables charged particles to rapidly enter a capillary tube and be concentrated into a narrow sample zone. The equilibrium of equation 2 is broken and more analyte is protonated, resulting in the continual transfer of analyte in the organic phase of equation 1 to the water column. Therefore, under a high electric field, on-line back extraction and field amplification sample injection can be simultaneously completed, and the direct high-sensitivity detection of capillary electrophoresis of substances in the water-immiscible solution is realized.
Drawings
The attached figure is a schematic structural diagram of the on-line back extraction one-field amplification sample feeding device provided by the invention.
In the figure, a capillary 1, a buffer solution 2, an anode 3, a sample tube 4, a water column 5, a phase interface 6, a sample 7, a water-immiscible solvent 8, a cathode 9 and a buffer solution bottle 10 are arranged
Detailed Description
The technical solution of the present invention will be further described with reference to specific examples.
As shown in the figure, the online back extraction-field amplification sample injection device mainly comprises a sample tube 4 and a capillary electrophoresis system, wherein the sample tube 4 is communicated with a buffer solution bottle 10 in the capillary electrophoresis system through a capillary 1, a water column 5 is used for encapsulating a solution immiscible with water in the sample tube 4 (the solution is formed by dissolving a sample 7 in a water immiscible solvent 8 in the figure), a separation capillary orifice of the capillary electrophoresis system is positioned in the water column 5, and an anode 3 and a cathode 9 are respectively inserted into the water column 5 of the sample tube 4 and the buffer solution 2 in the buffer solution bottle 10.
When the device is used for detection, a solution immiscible with water is sealed in a sample tube by a section of water column 5 (compared randomly), the solution immiscible with water and the water column are completely layered in the sample tube, namely, after a phase interface 6 appears, the sample tube is placed at a capillary electrophoresis sample injection position of a capillary electrophoresis system, a sample injection port of a separation capillary is ensured to be positioned in the water column, then sample injection voltage is applied, a sample extracted into the water column enters a buffer solution in a capillary column, an object to be detected in the solution immiscible with water is continuously transferred into the water column, finally, online back extraction and field amplification sample injection are simultaneously realized, and capillary electrophoresis direct detection of the substance in the solution immiscible with water is completed.
By using the device and solvent micro extraction together, the cocaine and thebaine in the urine sample can be detected by capillary electrophoresis-ultraviolet detection. The linear range of the detection result is 0.040-4 mug/ml; the detection limit of capillary electrophoresis-ultraviolet detection is 5-10ng/ml, and the detection sensitivity is high. The whole analysis operation can be completed within 15 minutes, and the method has the advantages of simplicity, convenience, rapidness and sensitivity.
Claims (2)
1. A method for directly detecting capillary electrophoresis of substances in water-immiscible solution is characterized in that firstly, the water-immiscible solution is sealed in a sample tube by a section of water column (compared randomly), after the water-immiscible solution and the water column are completely layered in the sample tube, the sample tube is placed at a capillary electrophoresis sample injection position of a capillary electrophoresis system, a sample injection port of a separation capillary is ensured to be positioned in the water column, then sample injection voltage is applied, a sample extracted into the water column enters a buffer solution in a capillary column, and a substance to be detected in the water-immiscible solution is continuously transferred into the water column, finally, online back extraction and field amplification sample injection are simultaneously realized, and the capillary electrophoresis direct detection of the substances in the water-immiscible solution is completed.
2. An on-line back-extraction one-field amplification sample injection device for the method for directly detecting substances in water-immiscible solution by capillary electrophoresis as claimed in claim 1, which is characterized in that: the device mainly comprises a sample tube and a capillary electrophoresis system, wherein the sample tube is communicated with a buffer solution bottle in the capillary electrophoresis system through a capillary, a water column is used for encapsulating a solution which is not mutually soluble with water in the sample tube, a separation capillary injection port of the capillary electrophoresis system is positioned in the water column, and an anode and a cathode are respectively inserted into the water column of the sample tube and the buffer solution in the buffer solution bottle.
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CN 200610018169 CN1804610A (en) | 2006-01-16 | 2006-01-16 | Method and apparatus for capillary electrophoresis direct detection of substance in water-immiscible solution |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
CN116223172A (en) * | 2023-03-16 | 2023-06-06 | 杭州瑞旭科技集团有限公司 | Method for extracting and measuring cosmetic compliance cutin softening component |
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2006
- 2006-01-16 CN CN 200610018169 patent/CN1804610A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
CN116223172A (en) * | 2023-03-16 | 2023-06-06 | 杭州瑞旭科技集团有限公司 | Method for extracting and measuring cosmetic compliance cutin softening component |
CN116223172B (en) * | 2023-03-16 | 2023-08-29 | 杭州瑞旭科技集团有限公司 | Method for extracting and measuring cosmetic compliance cutin softening component |
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