Preparation method and application of molecular imprinted polymer on silica surface for specifically adsorbing patulin

A surface molecular imprinting and patulin technology, which is applied in material separation, analysis materials, instruments, etc., can solve the problems affecting the speed and accuracy of patulin detection, so as to avoid the loss of recovery rate and reduce the consumption , sample processing simple effect

Inactive Publication Date: 2010-12-15
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the sample processing method of the traditional HPLC method and the co-existing interfering substance 5-hydroxymethylfurfural produced by heating and other factors in the product have seriously affected the speed and accuracy of patulin detection.

Method used

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  • Preparation method and application of molecular imprinted polymer on silica surface for specifically adsorbing patulin
  • Preparation method and application of molecular imprinted polymer on silica surface for specifically adsorbing patulin
  • Preparation method and application of molecular imprinted polymer on silica surface for specifically adsorbing patulin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Silica gel surface activation

[0041] Take 20 g of microporous silica gel, wash it with 10% hydrochloric acid for 6 hours under reflux, wash it with ion water until neutral, wash it with acetone to remove the organic matter in the silica gel, dry it at 10°C and store it in a desiccator filled with nitrogen.

[0042] (2) Preparation of APTS-silica gel, the reaction equation of its preparation method is as figure 1 Shown:

[0043] Take 2g of activated silica gel and disperse it in 25ml of toluene, add 1ml of APTS, stir and reflux at 105°C for 6h under nitrogen protection; filter after the reaction, wash with toluene and ether in turn, and vacuum dry at room temperature to constant weight.

[0044] (3) Preparation of ACPC

[0045] Add 10ml SOCl2 to the 100ml three-necked bottle containing 25ml of dichloromethane, connect the tail gas treatment device, and put it in an ice bath to stir and reflux. Take another 3g of ACPA, add it into 15ml of dichloromethane to form...

Embodiment 2

[0054] (1) Silica gel surface activation

[0055] The surface pretreatment method of silica gel is as follows: take 20g of microporous silica gel, soak it in 50% nitric acid for 24 hours, wash it with deionized water until it is neutral, wash it with acetone to remove the organic matter in the silica gel, dry it at 10°C and place it in a desiccator filled with nitrogen. save in .

[0056] (2) Preparation of APTS-silica gel

[0057] The preparation method is the same as in Example 1.

[0058] (3) Preparation of ACPA-silica gel

[0059] Add 1g APTS-silica gel, 0.2663g ACPA and 0.0232g DMAP (catalyst) to the 100ml three-neck bottle containing 20ml dimethylformamide (DMF), stir and reflux under ice bath under nitrogen protection until the system is cooled, then add 0.2156 g DCC as a dehydrating agent, after the system slowly rises to room temperature, react for 4h, the reaction equation is as follows Figure 4 shown. After the reaction is completed, filter, and wash the filte...

Embodiment 3

[0066] (1) Surface activation of silica gel, the preparation method is the same as in Example 2.

[0067] (2) Preparation of APTS-silica gel, the preparation method is the same as in Example 1.

[0068] (3) Preparation of ACPA-silica gel, the preparation method is the same as Example 2.

[0069] (4) Preparation of patulin molecularly imprinted polymer

[0070] Take 20ml of DMSO, 0.065g 2-hydroxynicotinic acid, 4.0mmol monomer trifluoromethacrylic acid (TFMAA), 3.54ml EDMA and 0.5g ACPA-silica gel in a 100ml three-necked bottle, plug a ball of cotton in the bottle mouth, 70 Stir and react at ℃ for 24 hours; filter and wash the obtained filter residue with chloroform-methanol (4:1, V / V) until the washing residue meets ethanol without precipitation; then reflux the filter residue with 10% ethanol for 6 hours to remove the template molecule 2- Hydroxynicotinic acid was finally washed with ethanol and ether, and vacuum-dried at room temperature to obtain patulin molecularly impri...

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Abstract

A preparation method and application of a molecular imprinted polymer on the silica surface for specifically adsorbing patulin belong to the technical field of bioassay. The method comprises the following steps: firstly pretreating the silica surface; siliconizing the silica surface to prepare APTS-silica and introducing amino groups; preparing ACPA-silica by dewatering and esterifying or an acyl chloride intermediate method and grafting an azo initiator on the silica surface; and finally taking the patulin analog 2-hydroxynicotinic acid as a template to replace molecules, taking acrylamide, methylacrylic acid, 4-vinyl pyridine and trifluoromethyl acrylic acid as the functional monomers and taking ethylene glycol dimethacrylate (EDMA) as a cross-linking agent to obtain the molecular imprinted polymer on the silica surface in acetonitrile and pyridine solvents by thermal initiation. The invention has the following advantages: as the pretreatment method for liquid chromatography of trace patulin in apple juice and related products, the polymer prepared by the invention can specifically adsorb the enriched patulin, the sample is simply and quickly treated and can be reused multiple times, and the polymer is resistant to acid and alkali treatment and is preserved under normal temperature, at the same time, the invention avoids the recovery loss caused by the traditional steps of removing impurities by alkaline washing by liquid-liquid extraction and removing organic solvents by rotary evaporation and reduces the usage amount of the organic solvents.

Description

technical field [0001] The present invention relates to a polymer preparation method and application in the technical field of biological detection, in particular to a silica gel surface molecularly imprinted Aspergillus clavus that can be used as liquid chromatography detection and analysis of trace patulin in apple juice and related products Preparation methods and applications of protein-specific polymers. technical background [0002] Patulin is mainly a toxic secondary metabolite produced by fungi such as Penicillium and Aspergillus. Recently, the detection technology of patulin in apple juice has become a research hotspot at home and abroad because of its toxic and side effects. For example, Chinese patent application number: CN03160299.1 is found according to retrieval, title: method and application of patulin immunochromatographic detection test paper, and the technology is called: rapid detection method. The detection test paper of the invention includes a liner, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F2/44C08F4/04C08J9/26G01N30/02G01N30/06
Inventor 赵大云于学雷贾竞夫
Owner SHANGHAI JIAO TONG UNIV
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