Synthesis and Application of Chitosan Immobilized Cyclodextrin Phosphorylated Double Modified Derivatives

A technology of cyclodextrin and chitosan, which is applied in the field of synthesis of chitosan-immobilized cyclodextrin phosphorylated double-modified derivatives, can solve the problems of high price, high technical operation requirements, and low algal toxin adsorption

Active Publication Date: 2017-10-17
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods are either time-consuming, require high technical operations, or are expensive, have low adsorption capacity for algal toxins, or have low specificity for microcystins, resulting in the accumulation and purification of microcystins. The purity is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Synthesis of Chitosan Immobilized Cyclodextrin Phosphorylated Double Modified Derivatives

[0033] The first step of preparation of mono-(6-p-tolylsulfonyl)β-cyclodextrin

[0034] Add 55g of β-CD into 435mL of distilled water, slowly add 5.2g of NaOH dissolved in distilled water into the suspension of β-CD, stir while adding dropwise, the time of dropping is 8~10min, and finally β-CD is completely dissolved In NaOH, the suspension became a clear solution of β-CD. Then, 24 mL of acetonitrile dissolved with 7.96 g of p-toluenesulfonyl chloride was added dropwise to the transparent β-CD solution, and stirred with a glass rod while adding, and the dropping time was 10 to 12 minutes. After the dropwise addition, the transparent β-CD solution became cloudy. Then stir at 1000r / min for 2.5h on a constant temperature magnetic stirrer at 22°C. After the reaction, the supernatant was obtained by centrifugation, and the supernatant was placed at 4°C for half a day, and a larg...

Embodiment 2

[0043] 1. Synthesis of Chitosan Immobilized Cyclodextrin Phosphorylated Double Modified Derivatives

[0044] The first step and the second step are with embodiment 1.

[0045] third step

[0046] The third step is the synthesis of chitosan-immobilized cyclodextrin phosphorylated double-modified derivatives (CTS-CD-P chitosan derivatives)

[0047] Dissolve 3g of chitosan immobilized cyclodextrin synthesized in 36mL of methanesulfonic acid solution, then add 15g of P 2 o 5 , the whole reaction at N 2 Under the protection of the glass rod with constant stirring, carried out in an ice bath (0-5 ° C), by changing the reaction time or P 2 o 5 Phosphorylated chitosan with different degrees of substitution was obtained. After the reaction was completed, diethyl ether was added to precipitate the product, centrifuged, and the precipitate was washed with diethyl ether (5 times), acetone (3 times), methanol (3 times), and diethyl ether (1 time) respectively, and then freeze-dried. ...

Embodiment 3

[0053] 1. Synthesis of Chitosan Immobilized Cyclodextrin Phosphorylated Double Modified Derivatives

[0054] The first step and the second step are with embodiment 1.

[0055] third step

[0056] The third step is the synthesis of chitosan-immobilized cyclodextrin phosphorylated double-modified derivatives (CTS-CD-P chitosan derivatives)

[0057] Dissolve 2g of chitosan immobilized cyclodextrin synthesized in 14ml of methanesulfonic acid solution, then add 2g of P 2 o 5 , the whole reaction at N 2 Under the protection of the glass rod with constant stirring, carried out in an ice bath (0-5 ° C), by changing the reaction time or P 2 o 5 Phosphorylated chitosan with different degrees of substitution was obtained. After the reaction was completed, diethyl ether was added to precipitate the product, centrifuged, and the precipitate was washed with diethyl ether (5 times), acetone (3 times), methanol (3 times), and diethyl ether (1 time) respectively, and then freeze-dried. ...

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Abstract

The invention discloses a method for synthesizing chitosan immobilized cyclodextrin phosphorylated double-modified derivatives, which comprises the following steps: dissolving chitosan immobilized cyclodextrin in methanesulfonic acid, adding P2O5 under nitrogen protection, React in an ice bath. After the reaction, add ether to precipitate the product, and obtain chitosan-immobilized cyclodextrin phosphorylated double-modified derivatives. In the present invention, chitosan is selected as a carrier, and β-cyclodextrin is immobilized and phosphorylated to synthesize chitosan-immobilized cyclodextrin phosphorylated derivatives (CTS-CD-P). The derivatives specifically bind microcystins through cyclodextrin and thiol phosphate on chitosan, which improves the enrichment and adsorption efficiency of MC‑LR.

Description

technical field [0001] The invention belongs to the field of analysis of trace organic matter in water bodies and food grades, and relates to the preparation and use of chitosan-modified materials that specifically adsorb microcystins, in particular to a chitosan-immobilized cyclodextrin phosphoric acid Synthesis and application of double modified derivatives. Background technique [0002] With the acceleration of my country's modernization process, harmful cyanobacterial blooms caused by surface water eutrophication often occur on a large scale, among which Microcystis blooms are the most common, and the produced microcystins are not only Seriously endanger fresh water bodies. In the food chain of fresh water ecological environment, algae cells containing microcystin are ingested by zooplankton, crustaceans, shellfish, etc., and enriched in various fish and other aquatic products and poultry through animal ingestion Meat products can cause damage to multiple organs of humans...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/24B01J20/30C08B37/08B01D15/08G01N30/02
Inventor 王海英赵晖梁晓声王朝元甘科
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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