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Preparation method and application of ractopamine molecularly-imprinted materials

A ractopamine and molecular imprinting technology, applied in analytical materials, material separation, chemical instruments and methods, etc., can solve the problems of too deep embedding of template molecules, irregular shapes, low mechanical properties, etc., and achieve adsorption equilibrium in a short time. The effect of high binding affinity and short elution time

Inactive Publication Date: 2012-07-18
NINGBO ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bulk polymerization method is currently the most widely used and the most mature and versatile method for preparing imprinted polymers. Its remarkable advantages are that the preparation process is relatively simple and the polymerization system is easy to control. Disadvantages such as leakage, irregular shape, and low mechanical properties have largely inhibited the application in real samples.
[0004] There are also literature disclosures in the prior art, such as the application number 200810153837.4 "A Preparation Method of High Molecular Polymers Enriched with Traces of Ractopamine" (publication number CN101747513A) discloses a method for preparing a molecular imprint of ractopamine, According to the paper "Molecularly imprinted polymer for the determination of trace ractopamine in pork using SPE followed by HPLC with fluorescence detection" published abroad by the applicant of the above application (Journal of Separation Science, 2009.9), it is known that the molecularly imprinted polymer prepared by surface imprinting method The adsorption amount of the compound for ractopamine is 1.99mg / g, which is relatively small, and further information is to be provided.

Method used

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  • Preparation method and application of ractopamine molecularly-imprinted materials
  • Preparation method and application of ractopamine molecularly-imprinted materials
  • Preparation method and application of ractopamine molecularly-imprinted materials

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh 30 g of silica gel (particle size 5 μm), add 150 mL of 10% (v / v) 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 50mL of xylene and 2mL of water, add 7mL of γ-chloropropyltrimethoxysilane, stir and react at 80°C for 8h, wash the product with water, and dry at 65°C for 12h to obtain double-bonded silica gel . Add 50mL of 50% by weight polyethyleneimine aqueous solution with a molecular weight of 10000, 3g of CP-SiO 2 , stirred at 80°C for reaction, and the adsorption material was obtained after 8 hours. After washing with water, dry at 65°C for 12 hours before use. Take 50mL concentration as 500mg·L -1 ractopamine aqueous solution, add 1g of adsorbent material, stir for 1h, so that the adsorption of ractopamine by the adsorbent material reaches saturation, adjust the pH value of the system to make pH = 8...

Embodiment 2

[0037]Weigh 30 g of silica gel (particle size 40 μm), add 150 mL of 20% (v / v) hydrochloric acid aqueous solution, stir at reflux temperature for 8 hours, wash with distilled water until neutral, and dry at 65°C for 12 hours to obtain activated silica gel. Add 5g of activated silica gel to 50mL of xylene and 2mL of water, add 7mL of γ-bromopropyltrimethoxysilane, stir and react at 90°C for 8h, wash the product with water, and dry at 65°C for 12h to obtain a double-bonded silica gel . Add 50mL 50% polyethyleneimine aqueous solution with a molecular weight of 20000, 3g CP-SiO 2 , Stir at 80°C to react, and get the adsorption material after 8h. After washing with water, dry at 65°C for 12 hours before use. Take 50mL concentration to be 800mg·L -1 ractopamine aqueous solution, add 1g of adsorbent material, stir for 1h, so that the adsorption of ractopamine by the adsorbent material reaches saturation, adjust the pH value of the system to make pH = 9.0, add 0.2mL of ethylene glyc...

Embodiment 3

[0039] Weigh 30 g of silica gel (particle size 120 μm), add 150 mL of 10% (v / v) 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 50mL of xylene and 2mL of water, add 7mL of γ-chloropropyltrimethoxysilane, stir and react at 80°C for 8h, wash the product with water, and dry at 65°C for 12h to obtain double-bonded silica gel . Add 50mL50% polyethyleneimine aqueous solution with a molecular weight of 50000, 3g CP-SiO2 to the flask 2 , stirred at 90°C for reaction, and the adsorption material was obtained after 8 hours. After washing with water, dry at 65°C for 12 hours before use. Take 50mL concentration as 1000mg·L -1 ractopamine aqueous solution, add 1g of adsorbent material, stir for 1h, make the adsorption of ractopamine by the adsorbent material reach saturation, adjust the pH value of the system to make pH = 10.0, ...

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Abstract

The invention discloses a preparation method of ractopamine molecularly-imprinted materials, and is characterized by comprising the following steps: (1) the activation of silica gel: weighing silica gel, and carrying out backflow activation on the silica gel by using an acidic aqueous solution; (2) the double-bond bonding of the silica gel: after the activated silica gel and a double-bond containing silane coupling agent are heated, and carrying out a reaction on the two; (3) the surface chemical grafting of the silicon gel: putting the silica gel into a polyethylenimine aqueous solution to carry out a heating reaction to obtain an adsorbing material; and (4) product preparation: adding the adsorbing material into a ractopamine aqueous solution, adjusting the system pH value of the obtained mixture to an alkaline value, adding a crosslinking agent in the alkaline mixture, and carrying out a heating reaction on the alkaline mixture; and after the heating reaction is completed, washing off template molecule ractopamine, and drying the obtained object so as to obtain a ractopamine molecularly-imprinted material. Compared with the prior art, the preparation method disclosed by the invention has the advantages that the method is simple in preparation process, strong in maneuverability and low in preparation cost; and the prepared molecularly-imprinted material is good in specificity, short in adsorption equilibrium time to ractopamine, short in elution time and good in elution effect.

Description

technical field [0001] The invention relates to a method for preparing a ractopamine molecularly imprinted material, and also relates to an application of the ractopamine molecularly imprinted material. Background technique [0002] Ractopamine (Rac) is a phenylethanolamine β-receptor agonist, which can improve the feed conversion rate and carcass lean meat rate in farming, and it has been approved as a feed additive in the United States. However, ractopamine metabolites are easy to accumulate in the body, and under excessive conditions, they can cause muscle tremors, tachycardia, arrhythmia, dizziness and other toxic and side effects to the human body. The application of β-receptor agonists such as clenbuterol and ractopamine in animal production is prohibited. However, driven by economic interests, illegal use of ractopamine still occurs from time to time. Therefore, in order to ensure food safety and human health, its monitoring is very important. Liquid-liquid partiti...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30G01N1/34G01N1/40G01N30/06
Inventor 杨挺吴银良吕燕叶宇飞
Owner NINGBO ACAD OF AGRI SCI
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