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Solid-phase micro-extraction column, and preparation and application methods thereof

A solid-phase microextraction column and conductive fiber technology, applied in the field of analytical chemistry, can solve the problems of accurate quantification of unfavorable analytes, tailing of analyte chromatographic peaks, bending of extraction columns, etc. Chromatographic analysis, high extraction efficiency, thickness controllable effect

Active Publication Date: 2020-12-01
HUBEI UNIVERSITY OF MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this technical solution has the following defects: 1) this technical solution needs to carry out electropolymerization in a relatively high concentration of strongly acidic supporting electrolyte solution, and the prepared extraction column has a good effect only on the enrichment of sulfa drugs; 2) online elution The extraction column may be bent or broken during the process; 3) Elution is performed with mobile phase, resulting in severe tailing of the analyte chromatographic peak, which is not conducive to the accurate quantification of the analyte

Method used

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  • Solid-phase micro-extraction column, and preparation and application methods thereof
  • Solid-phase micro-extraction column, and preparation and application methods thereof
  • Solid-phase micro-extraction column, and preparation and application methods thereof

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preparation example Construction

[0026] see figure 1 Shown, the present invention also provides a kind of preparation method of solid-phase microextraction column, it is characterized in that, comprises the following steps:

[0027] Step S1. Prepare a mixed solution of sodium hydroxide water-methanol (1:1, V / V) containing 0.01 to 0.5 mol / L of 2-mercaptobenzimidazole, or 0.01 to 0.5 mol / L of 2-mercaptobenzene A sulfuric acid aqueous solution with a concentration of imidazole of 0.01-0.05 mol / L is used as a supporting electrolyte solution.

[0028] Step S2. Take a bundle of conductive fibers, wash them successively with perchloric acid, sodium hydroxide solution, first-grade water, and methanol, and then dry them; specifically, the concentration of the sodium hydroxide solution is 0.01-0.2 mol / L.

[0029] Step S3. Take 5-50 mL of the solution obtained in step S1 and add it to the test tube as a supporting electrolyte solution;

[0030] Step S4. Wrap one end of the conductive fiber obtained in step S2 with tin...

Embodiment 1

[0036] 1) Prepare an aqueous solution containing 50% methanol (containing 0.01 to 0.5 mol / L of 2-mercaptobenzimidazole and 0.1 mol / L of sodium hydroxide), sonicate for a certain period of time to completely dissolve 2-mercaptobenzimidazole, and then pass Into nitrogen for 10 minutes to remove dissolved oxygen in water;

[0037] 2) Take a bundle of carbon fibers, wash them successively with perchloric acid, sodium hydroxide solution, first-grade water, and methanol, and then dry them;

[0038] 3) Take 5-50 mL of the solution obtained in step 1) and add it into a test tube as a supporting electrolyte solution;

[0039]4) Wrap one end of the carbon fiber with tin foil and fix it on the working electrode clip of the three-electrode system, and immerse the other end in the supporting electrolyte solution, and use cyclic voltammetry to electropolymerize with a certain potential range and scan rate under magnetic stirring state One layer of poly 2-mercaptobenzimidazole film is remov...

Embodiment 2

[0046] 1) Prepare an aqueous sulfuric acid solution containing 0.01-0.5 mol / L 2-mercaptobenzimidazole with a concentration of 0.01-0.05 mol / L as a supporting electrolyte solution. Ultrasound for a certain period of time to completely dissolve 2-mercaptobenzimidazole, and then pass nitrogen gas for 10 minutes to remove dissolved oxygen in the water;

[0047] 2) Take a bundle of fine copper wire fibers, wash them successively with perchloric acid, sodium hydroxide solution, first-grade water, and methanol, and then dry them;

[0048] 3) Take 20 mL of the solution obtained in step 1) and add it to the test tube as a supporting electrolyte solution;

[0049] 4) Wrap one end of the fine copper wire fiber with tin foil, fix it on the working electrode clip of the three-electrode system, and immerse the other end in the supporting electrolyte solution, and use cyclic voltammetry under a magnetic stirring state to scan Polymerize a layer of poly 2-mercaptobenzimidazole film at a high...

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Abstract

The invention discloses a solid-phase micro-extraction column, and preparation and application methods thereof, belonging to the technical field of analytical chemistry. The solid-phase micro-extraction column comprises a PEEK tube, wherein the PEEK tube is filled with a conductive fiber bundle, and the surface of the conductive fiber bundle is uniformly modified with a poly(2-mercaptobenzimidazole) membrane. The preparation method is simple and environmentally friendly; and a prepared coating is uniform and compact, controllable in thickness and free of obvious falling phenomenon after long-time use. The prepared poly(2-mercaptobenzimidazole)-modified carbon fiber-filled solid-phase micro-extraction column has a very good enrichment effect on resveratrol compounds, is combined with liquidchromatography in an off-line manner, and is suitable for enrichment and determination of resveratrol substances in plant tissues, food and other samples.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a solid-phase microextraction column and a preparation and application method thereof. Background technique [0002] Carbon Fiber (CF for short) is a high-strength new fiber material with a carbon content of more than 95%, and the diameter of a single fiber can reach 5-8 microns. It is a microcrystalline graphite material obtained by stacking structural units such as flake graphite microcrystals along the axial direction of the fiber, and is obtained by carbonization and graphitization, so it has good electrical conductivity. It has the strong tensile properties of carbon materials and the soft and processable properties of textile fibers. At the same time, the surface of carbon fibers is easy to handle, and the tip has certain mechanical strength and flexibility. The distance between each layer of carbon fiber is about 3.39 to 3.42 angstroms. The arrangement of car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/10G01N30/02G01N30/06
CPCB01D15/10G01N30/02G01N30/06G01N2030/062
Inventor 凌旭赵永恒戈振凯蒙静雯邱靖然薛雪梅
Owner HUBEI UNIVERSITY OF MEDICINE
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