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Preparation method and use of molecular imprinting-absorbing extraction stirring rod

A molecular imprinting and stirring rod technology, applied in selective adsorption, chemical instruments and methods, ion exchange, etc., can solve the problems of low coating selectivity and single type of coating, achieve uniform coating, improve accuracy and Precision, effectiveness in avoiding competing adsorption problems

Inactive Publication Date: 2009-12-02
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the limitations of the existing adsorption and extraction stirring rods with single coating types and low coating selectivity, and provide a new method for preparing molecularly imprinted adsorption and extraction stirring rods. The technical problems to be solved It uses molecular imprinting technology to prepare highly selective molecularly imprinted adsorption and extraction stirring rods, which directly use glass capillary as the substrate, built-in magnetic cores, and bond molecularly imprinted polymer coatings to prepare molecularly imprinted adsorption and extraction stirring rods. The method is simple, the material is easy to obtain, and the practicability is strong

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  • Preparation method and use of molecular imprinting-absorbing extraction stirring rod
  • Preparation method and use of molecular imprinting-absorbing extraction stirring rod
  • Preparation method and use of molecular imprinting-absorbing extraction stirring rod

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preparation example Construction

[0028] The preparation technology of the present invention is as follows:

[0029] Clean the inner and outer surfaces of the glass capillary with an inner diameter of 0.9-1.1 mm with tap water, then with distilled water, and dry in an oven at 120°C.

[0030]The pretreatment method of molecularly imprinted adsorption and extraction stirring rod substrate: sinter one end of the capillary on the flame of an alcohol lamp, then vertically insert it into a 1mol / L sodium hydroxide solution and soak for 8 hours, take it out and clean it with distilled water, and then vertically insert it into a 1mol / L sodium hydroxide solution Soak in hydrochloric acid solution for 1 hour, take it out, wash it with distilled water, and then wash it with methanol, then place it in an oven at 150°C for 1 hour, and cool it to room temperature for later use. Insert the activated capillary vertically into a 1:3 (v / v) diluted 3-methacryloyl-propyl-trimethoxysilane acetone solution, place it for 3-4 hours, p...

Embodiment 1

[0035] Preparation of Stir Bar for Molecularly Imprinted Adsorption and Extraction of Ractopamine:

[0036] Weigh 405.0 mg of ractopamine powder, dissolve it in 20.0 mL of methanol, add 0.4 mL of methacrylic acid, mix well, and place at room temperature for 12 hours. Add 4.6mL of ethylene glycol dimethacrylate, then add 45.9mg of azobisisobutyronitrile, mix well, ultrasonically degas for 5 minutes, take 1.5mL of the above prepolymerization solution in a test tube, put a silanized Reagent-treated glass capillaries are then purged with nitrogen to remove oxygen. The test tube was sealed with a rubber stopper and heated in a water bath at 60°C in a nitrogen blowing apparatus. After the polymerization reaction was carried out for 2.5 hours, the polymer solution was nearly solidified, and the glass capillary was pulled out vertically, and dried with nitrogen gas, and the polymerization was continued in a 60°C water bath for 24 hours after purging nitrogen gas to remove oxygen. Th...

Embodiment 2

[0045] Preparation of Stir Bar for Molecularly Imprinted Adsorption and Extraction of Terbutyzine:

[0046] Weigh 459.6 mg of terbutyzine powder, dissolve in 20.0 mL of toluene, add 0.7 mL of methacrylic acid, mix well, and place at room temperature for 12 hours. Add 2.6mL of trimethylolpropane trimethacrylate, then add 26.4mg of azobisisobutyronitrile, mix evenly, degas by ultrasonic for 5min, take 1.5mL of the above prepolymerization solution in a test tube, put it into a The glass capillary treated with silylating reagent was then purged with nitrogen to remove oxygen. The test tube was sealed with a rubber stopper and heated in a water bath at 60°C in a nitrogen blowing apparatus. After the polymerization reaction was carried out for 2 hours, the polymer solution was nearly solidified, the glass capillary was pulled out vertically, and dried with nitrogen gas, and the polymerization was continued in a 60°C water bath for 24 hours after purging nitrogen gas to remove oxyge...

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Abstract

The invention belongs to the technical field of sample pretreatment in analytical chemistry and relates to a preparation method and use of a molecular imprinting-absorbing extraction stirring rod. The preparation process of the method comprises the following steps: sintering one end of a capillary glass tube serving as a substrate of the stirring rod, and subjecting to the sintered capillary glass tube to acid and alkali treatment and surface modification by a silylating agent respectively; performing the self-assembly of template molecules and bifunctional monomers in a polymer solvent, adding a crosslinker and an initiator in the solution, plugging the modified capillary glass tube into the solution; drawing the capillary glass tube out; repeatedly coating the capillary glass tube to a required thickness, and aging the coating; cutting a proper length of coated capillary glass tube, putting the length of coated capillary glass tube in a magnetic core, and sintering the capillary glass tube for end sealing; and eluting the template molecules. The molecular imprinting-absorbing extraction stirring rod prepared by the invention can selectively separate and enrich a trace amount of template molecules and analogues at the same time and is suitable for selectively separating, enriching and analyzing a trace amount of template molecules and analogues in complex samples in terms of organism, food and environment.

Description

technical field [0001] The invention belongs to the technical field of analytical chemical sample pretreatment, and relates to a preparation method of a molecularly imprinted adsorption and extraction stirring rod, which is suitable for the pretreatment of complex samples such as food, biology and environment, and can be used for the separation and enrichment of imprinted molecules and their structural analogues. collection and trace analysis. Background technique [0002] The analysis of trace components in complex samples increasingly relies on fast, efficient, and selective sample pretreatment techniques. Traditional sample pretreatment techniques such as liquid-liquid extraction, Soxhlet extraction, solid-phase extraction and other extraction methods are time-consuming and cumbersome, have poor selectivity, and use a large amount of organic solvents. Molecularly imprinted polymers have specific recognition ability, can selectively separate and enrich the target, reduce ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08
Inventor 李攻科许志刚李家威胡玉玲
Owner SUN YAT SEN UNIV
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