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Method for purifying sulfanilamide drug by using molecularly imprinted polymer

A sulfonamide drug, molecular imprinting technology, applied in separation methods, chemical instruments and methods, organic chemistry, etc., can solve the problems of complex matrix interference, restricted development, non-specificity, etc., and achieves good specificity, improved sensitivity, and high capacity. Effect

Inactive Publication Date: 2012-02-08
SHANGHAI ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the non-specific interaction between the commonly used solid-phase extraction filler and the adsorption target, the selectivity of the stationary phase is low, and it is easily interfered by complex matrices, which limits the development of this technology.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Preparation of sulfa drug molecularly imprinted polymer:

[0025] Mix 0.6 mol of sulfonamide (template mixture), monomer methacrylic acid (MAA), and cross-linking agent ethylene glycol dimethacrylate (EGDMA) in a molar ratio of 1:2:20, dissolve to 2.5ml until Pore ​​agent (acetonitrile: methanol = 3: 2), placed in an ampoule, then added 0.02 g of initiator azobisisobutyronitrile (AIBN), ultrasonicated for 5 minutes, then flushed with nitrogen for 5 minutes, vacuum sealed, 60 In a water bath for 24 hours, the sulfonamide molecularly imprinted polymer was obtained. Take out the blocky polymer, grind it with a mortar, sieve it to an average particle size of 30-60 μm, suspend it with acetone and discard the fine particles. After the polymer was dried, the template was removed by Soxhlet extraction with methanol (containing 10% acetic acid) for 72 hours, and the medium was changed every 8 hours. Take 20 ul of the eluent, and after HPLC determines that the elution is com...

Embodiment 2

[0032] 1. Preparation of molecularly imprinted polymers:

[0033]With template mixture 0.6mol, monomer methacrylic acid (MAA), cross-linking agent ethylene glycol dimethacrylate (EGDMA), mix according to the molar ratio of 1:4:20, dissolve into 5ml porogen (acetonitrile :methanol=3:2), put it into an ampoule bottle, then add 0.02g of initiator azobisisobutyronitrile (AIBN), ultrasonic for 5 minutes, then flush with nitrogen for 5 minutes, vacuum seal, and place in a 60-degree water bath for 36 hours , to obtain molecularly imprinted polymers. Take out the blocky polymer, grind it with a mortar, sieve it to a particle size of 30-60 μm, suspend it with acetone and discard the fine particles. After drying the polymer, use methanol (containing 10% acetic acid) for Soxhlet extraction for 48 hours to remove the template and change the solution every 8 hours. After the elution was determined by HPLC, it was dried at 60°C for 24 hours for later use.

[0034] 2. Preparation of sulfo...

Embodiment 3

[0040] 1. Preparation of sulfonamide molecularly imprinted polymer:

[0041] 0.6mol of template mixture, monomer methacrylic acid (MAA), and crosslinking agent ethylene glycol dimethacrylate (EGDMA) were mixed according to the molar ratio of 1:3:20, and dissolved in 3ml porogen (acetonitrile :methanol=3:2), put it into an ampoule bottle, then add 0.02g of initiator azobisisobutyronitrile (AIBN), ultrasonication for 10 minutes, then flush with nitrogen for 5 minutes, vacuum seal, and place in a 65-degree water bath for 24 hours , to obtain molecularly imprinted polymers. Take out the blocky polymer, grind it with a mortar, sieve it to a particle size of about 30-60 μm, suspend it with acetone and discard the fine particles. After the polymer was dried, the template was removed by Soxhlet extraction with methanol (containing 10% acetic acid) for 24 hours. After the elution was determined by HPLC, it was dried at 60°C for 24 hours for later use.

[0042] 2. Preparation of Mole...

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Abstract

The present invention belongs to the technical field of bioengineering, and relates to a method for purifying sulfanilamide by using a molecularly imprinted polymer of a sulfanilamide drug. The method comprises the following steps: (1) mixing and dissolving template molecules of a sulfanilamide drug mixture, a functional monomer of methacrylic acid and a cross-linking agent of ethylene glycol dimethacrylate in a pore forming agent (a ratio of methanol to acetonitrile is 2:3); adding an initiator, and sealing; (2) crushing the synthesized polymer, removing fine particles, removing the template molecules through extraction; (3) drying the template molecule-removed polymer overnight at a temperature of 60 DEG C to obtain the molecularly imprinted polymer of the sulfanilamide; (4) filling the molecularly imprinted polymer into a solid phase extraction column tube; (5) activating the solid phase extraction column, adding an animal tissue extraction solution or a water sample, wherein the animal tissue extraction solution is dissolved in 40% methanol; then leaching the solid phase extraction column to elute and purify the sulfanilamide. The method provided by the present invention has advantages of high selectivity, high specificity and adverse environment resistance, and has broad application potential.

Description

technical field [0001] The invention relates to a method in the technical field of biochemical engineering, specifically, a method for purifying sulfonamide drugs by using molecularly imprinted polymers. Background technique [0002] Sulfonamides, a widely used drug for humans and animals, can interfere with the utilization of para-aminobenzoic acid by bacteria, thereby affecting the synthesis of bacterial DNA. May cause residue if used incorrectly. Because sulfa drugs have a long metabolism time in animals, it is easy to cause drug residues in the body. The harmfulness of sulfonamide drug residues is manifested in the following aspects: it can cause allergic reactions in the body; induce the production of drug-resistant strains; infringe on the nervous system, thereby affecting the intellectual development of offspring; destroy the hematopoietic system of the body, causing various In addition, the residues of sulfonamides have strong carcinogenic, teratogenic and mutageni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08F2/44C08J9/28B01D15/22B01J20/285C07D239/69C07D261/16
Inventor 宋素泉赵志辉姚春霞
Owner SHANGHAI ACAD OF AGRI SCI
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