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Dextran gel integral adsorption extraction stirring rod and preparation method and application thereof

A technology of dextran gel and stirring rod, which is applied in the field of analytical chemistry, can solve the problems that the weight of the stirring rod is difficult to provide magnetic force, the magnetic force of the stirring rod is insufficient for adsorption and extraction, and the thickness of the coating is limited, so as to improve the reusability and stability Sexuality, fast and efficient enrichment, and the effect of improving magnetic and mechanical stability

Active Publication Date: 2019-02-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

SBSE is prepared by immobilizing the polymer coating on the outer layer of the capillary glass capillary with the built-in magnetic core. The coating is mainly non-specific adsorption coating such as polydimethylsiloxane and heat-resistant engineering plastic polyether. Sulfone ketone PPESK, etc., the selectivity is not high, and the coating thickness is limited and may fall off or be damaged
The outside of the stirring rod is coated, and the inside is an iron core. It is difficult to provide enough magnetic force when the stirring rod is heavy
[0004] Therefore, there is an urgent need to research and develop an integral adsorption extraction stirring rod and its preparation method and its use in the extraction and detection of target substances in complex samples, so as to overcome the low specificity and poor specificity in the enrichment process of the existing SBSE extraction technology. Insufficient magnetic force of adsorption and extraction stirring bar

Method used

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  • Dextran gel integral adsorption extraction stirring rod and preparation method and application thereof
  • Dextran gel integral adsorption extraction stirring rod and preparation method and application thereof
  • Dextran gel integral adsorption extraction stirring rod and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0062] 1. Magnetic powder for dextran modification pretreatment:

[0063] (1) Pretreatment of magnetic powder: Soak superparamagnetic NdFeB magnetic powder in acetone solution for 30 minutes, wash it with deionized water, and then soak it in 1mol / L sodium hydroxide solution at 80°C for 20 minutes to remove the surface of the magnetic powder Organic matter, vacuum dried after washing with deionized water;

[0064] (2) Dextran-modified pretreatment of magnetic powder: first prepare sodium hydroxide / diethylene glycol mixture, add 100mmol sodium hydroxide to 40mL diethylene glycol, stir and heat until the sodium hydroxide is completely dissolved and store at 70°C. Add 2g of the treated magnetic powder and 5g of dextran gel into 200mL of diethylene glycol, stir well at 210°C and slowly add 20mL of the above-mentioned sodium hydroxide / diethylene glycol mixture, react at 210°C for 2h, and cool the products separately Rinse with ethyl acetate, ethanol, and deionized water, dry in vac...

Embodiment 2

[0081] 1. Magnetic powder for dextran modification pretreatment:

[0082] (1) Pretreatment of magnetic powder: Soak superparamagnetic NdFeB magnetic powder in acetone solution for 30 minutes, wash it with deionized water, and then soak it in 1mol / L sodium hydroxide solution at 80°C for 20 minutes to remove the surface of the magnetic powder Organic matter, vacuum dried after washing with deionized water;

[0083] (2) Dextran-modified pretreatment of magnetic powder: first prepare sodium hydroxide / diethylene glycol mixture, add 80mmol sodium hydroxide to 40mL diethylene glycol, stir and heat until the sodium hydroxide is completely dissolved and store at 70°C. Add 3g of the treated magnetic powder and 5g of dextran gel into 200mL of diethylene glycol, stir well at 210°C and slowly add 35mL of the above-mentioned sodium hydroxide / diethylene glycol mixture, react at 210°C for 2h, and cool the products separately Rinse with ethyl acetate, ethanol, and deionized water, dry in vacu...

Embodiment 3

[0097] Using the same preparation method and conditions as in Example 1, the only difference is that THF is 30wt%, dextran gel is 15wt%, thioglycolic acid is 25wt%, concentrated sulfuric acid is 0.1wt%, and the reaction temperature in step B is 40°C. The time is 60h; ethylene glycol dimethacrylate 30wt%, azobisisobutyronitrile 0.3wt%, mercaptodextran gel 10wt%, organic solvent 50wt%; ultrasonic time is 5min, the reaction temperature in step C 80°C, through the same detection as in Example 1, it was found that the stirring rod prepared in Example 3 had a good enrichment effect on the target substance, and the analysis had high sensitivity.

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Abstract

The invention relates to a dextran gel integral adsorption extraction stirring rod, which comprises a homogenous body of a mercapto-containing dextran gel and dextran-modified magnetic powder, and thehomogenous body contains a cavity matching a template molecule. The invention also relates to a preparation method of the dextran gel integral adsorption extraction stirring rod. The integral adsorption extraction stirring rod prepared by the interaction of the magnetic material and the dextran gel is the homogenous body, has high mechanical strength, and strong solvent resistance, the preparation method has simple and easy process and low cost, and the stirring rod can quickly and efficiently enrich the target substances.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a dextran gel integral adsorption extraction stirring rod and a preparation method and application thereof. Background technique [0002] Dextran gel is a polymer compound with a porous network structure that is cross-linked by straight-chain dextran molecules and a cross-linking agent. The size of the mesh in the gel particles can be controlled by adjusting the ratio of dextran and cross-linking agent. The larger the degree of cross-linking, the tighter the mesh structure; the smaller the degree of cross-linking, the looser the mesh structure. The size of the gel determines the molecular weight range in which the separated substance can freely enter and exit the gel. Dextran gel is hydrophilic, rich in ligands, easy to chemically modify, and is an ideal polymer support. In 1986, Wang Qichao et al first linked sulfhydryl groups to dextran gels to synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/282B01J20/30B01D15/22
CPCB01D15/22B01J20/282
Inventor 刘静黄文氢张明森
Owner CHINA PETROLEUM & CHEM CORP
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