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Preparation method of rare-earth fluorescent molecularly imprinted membrane and application of rare-earth fluorescent molecularly imprinted membrane

A molecularly imprinted membrane and rare earth fluorescence technology, applied in the field of preparation of rare earth fluorescent imprinted membrane, can solve the problems of poor selectivity of adsorbents, high cost, secondary pollution, etc., and achieve the effects of high sensitivity, reduction of detection time, and improvement of sensitivity

Inactive Publication Date: 2015-06-03
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, solvent extraction technology uses a large amount of organic solvents, which is prone to secondary pollution; although supercritical extraction has the advantages of easy separation of solvent and target and no pollution, the operation is complicated and costly; membrane separation technology has the problem of membrane clogging; Adsorbents commonly used in solid phase extraction techniques have poor selectivity

Method used

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  • Preparation method of rare-earth fluorescent molecularly imprinted membrane and application of rare-earth fluorescent molecularly imprinted membrane
  • Preparation method of rare-earth fluorescent molecularly imprinted membrane and application of rare-earth fluorescent molecularly imprinted membrane
  • Preparation method of rare-earth fluorescent molecularly imprinted membrane and application of rare-earth fluorescent molecularly imprinted membrane

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Experimental program
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Effect test

Embodiment 1

[0038] (1) EuCl 3 0.5 mmol, 0.75 mmol of phen, and 0.5 mmol of TTA were dissolved in 100 mL of ethanol, stirred evenly by magnetic force, and concentrated ammonia water was added dropwise. Adjust pH=7, the solution becomes turbid. Continue stirring for 2 h, centrifuge, and wash three times with ethanol. The Eu(III) complex is obtained.

[0039](2) Dissolve 100 mg of Eu(III) complex in step (1) in 5 mL of DMF. Form solution A with a mixed solution of 25 ml ethanol and 1 mL TEOS. Then 1 mL of ammonia water was added to the mixed solution of 14 ml of ethanol and 5 ml of distilled water to form solution B, then solution A was quickly poured into solution B, and magnetically stirred for 2 h. centrifuged and washed three times to obtain Eu(III)SiO 2 .

[0040] (3) Eu(III)SiO obtained in (2) 2 0.1 g was dispersed in 30 mL of acetonitrile, and then 0.35 mmol of methacrylic acid (MAA), 1.50 mL of ethylene glycol dimethacrylate (EGDMA), and 0.10 mmol of cyfluthrin were added. ...

Embodiment 2

[0045] (1) EuCl 3 0.5 mmol, 0.5 mmol of phen, and 0.5 mmol of TTA were dissolved in 100 mL of ethanol, stirred evenly by magnetic force, and concentrated ammonia water was added dropwise. Adjust pH=7, the solution becomes turbid. Continue stirring for 2 h, centrifuge, and wash three times with ethanol. The Eu(III) complex is obtained.

[0046] (2) Dissolve 20 mg of the Eu(III) complex in step (1) in 1 mL of DMF. Form solution A with a mixed solution of 5 ml ethanol and 0.19 mL TEOS. Then 0.2 mL of ammonia water was added to the mixed solution of 3.5 mL of ethanol and 1.3 mL of distilled water to form solution B, then solution A was quickly poured into solution B, and magnetically stirred for 2 h. centrifuged and washed three times to obtain Eu(III)SiO 2 .

[0047] (3) Disperse 0.12 g of the fluorescent material obtained in (2) in 30 mL of acetonitrile, and then add 0.50 mmol of methacrylic acid (MAA), 1.55 mL of ethylene glycol dimethacrylate (EGDMA), and 0.12 mmol of c...

Embodiment 3

[0053] (1) EuCl 3 0.5 mmol, 0.5 mmol of phen, and 0.5 mmol of TTA were dissolved in 100 mL of ethanol, stirred evenly by magnetic force, and concentrated ammonia water was added dropwise. Adjust pH=7, the solution becomes turbid. Continue stirring for 2 h, centrifuge, and wash three times with ethanol. The Eu(III) complex is obtained.

[0054] (2) Dissolve 50 mg of the Eu(III) complex in step (1) in 2 mL of DMF. The mixed solution with 10ml ethanol and 0.5 mL TEOS forms solution A. Then 0.4 mL of ammonia water was added to the mixed solution of 7 ml of ethanol and 2.5 ml of distilled water to form solution B, then solution A was quickly poured into solution B, and magnetically stirred for 2 h. centrifuged and washed three times to obtain Eu(III)SiO 2 .

[0055] (3) Disperse 0.12 g of the fluorescent material obtained in (2) in 30 mL of acetonitrile, and then add 0.60 mmol of methacrylic acid (MAA), 1.70 mL of ethylene glycol dimethacrylate (EGDMA), and 0.15 mmol of cyfl...

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Abstract

The invention belongs to the technical fields of material preparation, analysis and detection, and discloses a preparation method of a rare-earth fluorescent molecularly imprinted membrane and an application in detection of cyfluthrin. According to the technical scheme disclosed by the invention, the method comprises the following steps: preparing an Eu (III) rare-earth complex by a solution method; wrapping the rare-earth complex with a silicon-based surface; adopting a surface molecular imprinting technology; and with cyfluthrin as a template, methacrylic acid (MAA) as a functional monomer and EGDMA as a cross-linking agent and azobisisobutyronitrile (AIBN) as an initiator, preparing a rare-earth fluorescent molecularly imprinted probe. Trace cyfluthrin in a water sample is detected by a fluorescence analysis method; the related coefficient R2 is 0.99269; and the result proves that the rare-earth fluorescent molecularly imprinted probe obtained by the method has excellent recognition performance and extremely high sensitivity on cyfluthrin molecules.

Description

technical field [0001] The invention relates to a preparation method of a rare earth fluorescent imprinted film, in particular to a preparation method of a cyfluthrin molecular fluorescent imprinted film, and its application to detecting trace amounts of cyfluthrin in water, belonging to the technical field of material preparation and detection. Background technique [0002] Pyrethroid pesticides (PPs) are a class of artificially synthesized broad-spectrum insecticides, which have the characteristics of quick-acting, odorless, low toxicity, strong contact action and long residual time. In addition to having special effects on more than 140 kinds of pests, some pyrethroid pesticides also have good control effects on underground pests and acarid pests. In recent years, after the use of highly toxic organochlorine and organophosphorus pesticides was banned, PPs has a wider application space, and it has occupied nearly 20% of the international pesticide market. It is generally ...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08J9/26C08L33/02C08L5/12C08F220/06C08F222/14C08F2/44C08K9/04C08K9/06C08K3/36B01J20/281B01J20/28B01J20/30B01D15/08G01N21/64
Inventor 郑旭东汪纯戴江栋王吉祥卫潇闫永胜
Owner JIANGSU UNIV
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