Preparation method and application of phenylethanolamine A molecularly-imprinted material

A technology of phenylethanolamine and molecular imprinting, which is applied in the preparation of surface molecular imprinting materials capable of detecting residues of phenylethanolamine A, and in the application field of surface molecular imprinting materials, which can solve the problem of decreased sensitivity of the detection method, large impurity interference, and recovery of the accuracy of detection results. low efficiency and other problems, to achieve the effect of low preparation cost, short elution time and simple preparation process

Inactive Publication Date: 2012-07-04
NINGBO ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the detection work, low recovery rate or high impurity interference often occurs, which directly leads to a decrease in the accuracy of the detection results and the sensitivity of t

Method used

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  • Preparation method and application of phenylethanolamine A molecularly-imprinted material
  • Preparation method and application of phenylethanolamine A molecularly-imprinted material
  • Preparation method and application of phenylethanolamine A molecularly-imprinted material

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Embodiment 1

[0027] Weigh 30 g of silica gel (particle size 5 μm), add 150 mL of 10% methanesulfonic acid aqueous solution, stir at reflux temperature for 8 h, wash with distilled water until neutral, and dry at 65° C. for 12 h to obtain activated silica gel. Add 10g of activated silica gel to 400mL of water, add 10mL of 3-(methacryloyloxy)propyltrimethoxysilane, stir and react at 50°C for 24h, wash the product with water and ethanol, and dry at 65°C for 12h to obtain a double bond Composite silicone. Add 200mL of water and 3g of double-bonded silica gel into the flask, stir for 1h, then add 10mL of methacrylic acid, in N 2 Stir for 1 h under protection, add 1 mL of 20% ammonium persulfate solution, heat up to 70° C., stir for graft polymerization, and obtain grafted particles after 24 h. Soxhlet extraction with ethanol for 24 hours, and then dried at 65°C for 12 hours before use. Take 50mL concentration as 300mg·L -1 Aqueous solution of phenylethanolamine A, add 1g of grafted particles...

Embodiment 2

[0034] Weigh 30 g of silica gel (particle size 40 μm), add 150 mL of 10% methanesulfonic acid aqueous solution, stir at reflux temperature for 8 h, wash with distilled water until neutral, and dry at 65° C. for 12 h to obtain activated silica gel. Add 5g of activated silica gel to 200mL of water, add 5mL of 3-(methacryloyloxy)propyltrimethoxysilane, stir and react at 40°C for 24h, wash the product with water and ethanol, and dry at 65°C for 12h to obtain a double bond Composite silicone. Add 200mL of water and 3g of double-bonded silica gel into the flask, stir for 1h, then add 10mL of methacrylic acid, in N 2 Stir for 1 h under protection, add 1 mL of 10% ammonium persulfate solution, heat up to 70° C., stir for graft polymerization, and obtain grafted particles after 24 h. Soxhlet extraction with ethanol for 24 hours, and then dried at 65°C for 12 hours before use. Take 50mL concentration as 400mg·L -1 Aqueous solution of phenylethanolamine A, add 1g of grafted particles ...

Embodiment 3

[0036] Weigh 30 g of silica gel (particle size 120 μm), add 150 mL of 20% hydrochloric acid aqueous solution, stir at reflux temperature for 8 h, wash with distilled water until neutral, and dry at 65° C. for 12 h to obtain activated silica gel. Add 5g of activated silica gel to 200mL of water, add 5mL of 3-(methacryloyloxy)propyltrimethoxysilane, stir and react at 60°C for 24h, wash the product with water and ethanol, and dry at 65°C for 12h to obtain a double bond Composite silicone. Add 200mL of water and 3g of double-bonded silica gel into the flask, stir for 1h, then add 10mL of methacrylic acid, stir for 1h under the protection of N2, add 1mL of 10% ammonium persulfate solution, heat up to 70°C, and stir for graft polymerization , After 24h, the grafted particles were obtained. Soxhlet extraction with ethanol for 24 hours, and then dried at 65°C for 12 hours before use. Take 50mL concentration as 500mg·L -1 Aqueous solution of phenylethanolamine A, add 1g of grafted p...

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Abstract

The invention discloses a preparation method of a phenylethanolamine A molecularly-imprinted material, which is characterized by comprising the following steps of: (1) activating silica gel; (2) carrying out double-bond bonding on the silica gel; (3) carrying out chemical grafting on the surface of the silica gel and obtaining grafting particles; and (4) preparing the product: adding the grafting particles into 300-500mg/L phenylethanolamine A aqueous solution, adjusting the pH value of the system to be alkaline, adding a crosslinking agent and heating for reaction; after the reaction is finished, washing off template molecule phenylethanolamine A, drying and obtaining the phenylethanolamine A surface molecularly-imprinted material. Compared with the prior art, the preparation method has the advantages that the preparation process is simple, the operability is strong, and the preparation cost is low; and the molecularly-imprinted material is good in specificity, short in adsorption equilibrium time of phenylethanolamine A, short in elution time and good in elution effect.

Description

technical field [0001] The invention relates to a method for preparing a surface molecularly imprinted material, in particular to a method for preparing a surface molecularly imprinted material capable of detecting phenylethanolamine A residue. The invention also discloses the application of the surface molecular imprinting material. Background technique [0002] Phenylethanolamine A, also known as clonpamine, is a synthetic chemical substance that has the same action and effect as clenbuterol and ractopamine. In recent years, the presence of phenylethanolamine A has been found in feed and animal products. Humans will have serious side effects after eating food containing phenylethanolamine A. Long-term consumption of food containing phenylethanolamine A will cause diseases of the human cardiovascular system and nervous system, and even cause chromosomal aberrations and induce malignant tumors. The Ministry of Agriculture of my country issued Announcement No. 1519 in 2011,...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30G01N30/14
Inventor 吴银良杨挺陈国孙亚米
Owner NINGBO ACAD OF AGRI SCI
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