Method for preparing fudosteine molecularly imprinted polymer

A technology of molecular imprinting and polymers, which is applied in the fields of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of difficult degradation, residue, long metabolism time, etc., to improve detection sensitivity and The effect of detection efficiency and large promotion and application value

Inactive Publication Date: 2011-05-18
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because fudosteine ​​is not easy to degrade in the body, and the metabolism time is long, if it is us

Method used

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  • Method for preparing fudosteine molecularly imprinted polymer
  • Method for preparing fudosteine molecularly imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Mix fudosteine ​​0.5mmol, MAA1mmol, EGDMA10mmol, pour into 2.5ml of methanol and toluene mixture, the ratio of the two is 1:1.4, after standing at room temperature for half an hour, add 20mg of initiator AIBN.

[0019] Put the above mixture into a reaction bottle, and degas it by ultrasonic for 10 min. The degassed system was purged with nitrogen for 5 minutes to remove oxygen. Quickly seal under nitrogen protection. 55 ℃ water bath insulation reaction for 14h. The reaction product is obtained.

[0020] After the reaction, the prepared molecularly imprinted polymer was ground and passed through a sample sieve. After settling with acetone three times, the obtained polymer was dried, and the particle diameter of the polymer was between 30-60 um. Template molecules were removed by Soxhlet extraction for 12 h. The extraction reagent is 180mL methanol containing 10% acetic acid. Residual acetic acid was eluted with methanol. The molecularly imprinted polymer from whic...

Embodiment 2

[0022] Mix fudosteine ​​0.5mmol, MAA 2mmol, EGDMA 10mmol, pour into porogen methanol, toluene mixture 2.5mL, the ratio of the two is 1:1.4, after standing at room temperature for 1h, add initiator AIBN 20mg. Put the above mixture into a reaction bottle and degas it by ultrasonic for 5 min. The degassed system was purged with nitrogen for 5 minutes to remove oxygen. Quickly seal under nitrogen protection. 60 ℃ water bath insulation reaction for 24h.

[0023] After the reaction, the prepared molecularly imprinted polymer was ground, and the sample was sieved with a standard sieve. After the polymer was settled 3 times with acetone, the obtained polymer was dried. Template molecules were removed by Soxhlet extraction for 20 h. The extraction reagent is 180mL methanol containing 20% ​​acetic acid. Residual acetic acid was eluted 1-2 times with methanol. Finally, the molecularly imprinted polymer from which template molecules were removed was vacuum-dried overnight at 60° C. ...

Embodiment 3

[0025] Mix 0.5mmol of fudosteine, 4mol of MAA, and 10mmol of EGDMA, pour into 2.5mL of methanol and toluene mixture, the ratio of the two is 1:1.4, and after standing at room temperature for 1h, add 20mg of initiator AIBN. Put the above mixture into a reaction bottle, and degas it by ultrasonic for 10 min. The degassed system was purged with nitrogen for 10 minutes to remove oxygen. Seal quickly under the protection of nitrogen. 55 ℃ water insulation reaction for 20h.

[0026] After the reaction, the prepared molecularly imprinted polymer was ground and passed through a sample sieve. After settling through acetone 3 times, the resulting polymer was dried. The template molecules were removed by Soxhlet extraction for 36 h. The extraction reagent is 180ml methanol containing 30% acetic acid. Finally, the molecularly imprinted polymer from which template molecules were removed was dried overnight at 60° C. to obtain fudosteine ​​molecularly imprinted polymer. Electron micro...

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Abstract

The invention provides a method for preparing fudosteine molecularly imprinted polymer and belongs to the technical field of chemical engineering. The method comprises: dissolving fudosteine serving as template molecules, methacrylic acid serving as functional monomer and an ethylene glycol dimethacrylate serving as a cross-linking agent according to a molar ratio of 1:3-4:10, wherein a pore forming agent is mixed liquid of methanol and methylbenzene in a ratio of 1:1-3; adding azodiisobutyronitrile (AIBN) serving as an initiator; performing polymerization at 50 to 60 DEG C for 10 to 20 hours; milling the product, extracting with methanol-acetic acid solution for several times to remove template molecules, and drying at 60 DEG C and under vacuum to obtain fudosteine molecularly imprinted polymer. The fudosteine polymer prepared by the method can be used for detecting fudosteine residue in the environment or medicaments and the enrichment of trace amount of fudosteine, has the advantages of high speed, high flexibility, high accuracy, high yield, high repeatability and high sensitivity, and has a high application value and a bright market prospect.

Description

technical field [0001] The invention relates to a preparation method of fudosteine ​​molecularly imprinted polymer, which belongs to the field of new materials. Background technique [0002] Fudosteine ​​is a novel cysteine ​​derivative. Jointly developed by Japan SS Pharmaceutical Company and Welfide. In 2000, an oral preparation composition containing fudosteine ​​obtained an invention patent in Japan. In 2001, as a new drug mainly used to treat bronchitis and respiratory congestion, fudosteine ​​was first marketed in Japan. Currently, fudosteine ​​has been approved for recommended use in Australia. In 2003, a new oral preparation composition containing fudosteine ​​was granted an invention patent in China. However, since fudosteine ​​is not easy to degrade in the body and has a long metabolism time, if it is used improperly, it will cause residues, thus causing damage or pollution to humans, animals and the environment. In the 52-week safety evaluation study, researc...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F220/06C08F2/44C08J9/26B01J20/285B01J20/30B01J20/28
Inventor 刘冬青颜范勇董娇娇代林枫李爱梅
Owner TIANJIN POLYTECHNIC UNIV
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