Preparation and application of perfluorooctane sulfonic acid mesoporous molecularly imprinted fluorescent probe based on up-conversion material

A perfluorooctane sulfonate mesoporous and molecularly imprinted technology, applied in the field of molecularly imprinted fluorescent probes, can solve the problems of complicated instrument operation, limited application and popularization, expensive instruments, etc., achieve good selectivity, improve detection efficiency, reduce The effect of testing costs

Pending Publication Date: 2021-08-27
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although these analytical methods have good sensitivity, these instruments are relatively expensive and involve complicat

Method used

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  • Preparation and application of perfluorooctane sulfonic acid mesoporous molecularly imprinted fluorescent probe based on up-conversion material
  • Preparation and application of perfluorooctane sulfonic acid mesoporous molecularly imprinted fluorescent probe based on up-conversion material
  • Preparation and application of perfluorooctane sulfonic acid mesoporous molecularly imprinted fluorescent probe based on up-conversion material

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Experimental program
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Effect test

Embodiment 1

[0035] Preparation of PFOS mesoporous molecularly imprinted fluorescent probes for upconversion materials:

[0036] (1) Up-conversion material NaYF 4 : Yb, the preparation of Er: will contain the LnCl of 1mmol 3 (Ln=Y:Yb:Er, 80:18:2) 5mL aqueous solution was added to a 50mL beaker, then 2mmol sodium citrate and 10mL water were added, magnetically stirred for 10min, NaCl (2.88mmol) and NH 4 A 5 mL aqueous solution of F (6 mmol), OA (10 mL), and ethylene glycol (5 mL) were added to the above solution, and after stirring for 30 min, the mixed solution was transferred to a 50 mL reactor and reacted at 180°C for 6 h. After the reaction, use ethanol to centrifuge and wash 3 times, and finally place the obtained solid in a vacuum oven at 60°C for 6 hours to obtain the upconversion material NaYF 4 : Yb,Er(UCNPs).

[0037] (2) Preparation of amino-modified UCNPs: Weigh 100 mg of UCNPs into a 100 mL round bottom flask, add 10 mL of cyclohexane and 1 mL of IGEPALCO-520, and stir vigor...

Embodiment 2

[0040] Applications of PFOS mesoporous molecularly imprinted fluorescent probes for upconversion materials:

[0041]Add 800 μL molecularly imprinted fluorescent probe dispersion solution (0.05 g / L) and a certain volume of BR buffer solution in sequence into a 10 mL stoppered colorimetric tube, mix well, add a certain concentration of PFOS standard solution, and then use deionized water to set Make up to 10mL, react at room temperature for 10min, transfer to a cuvette after the reaction is complete, use a 980nm laser to excite, record the fluorescence emission spectrum and intensity of the system at 545nm, and realize the detection of PFOS according to the change value of the fluorescence intensity at 545nm Quantitative detection; PFOS combined with non-imprinted fluorescent probe experiments were carried out simultaneously under the same conditions.

Embodiment 3

[0043] Characterization of the PFOS mesoporous molecularly imprinted fluorescent probe of the up-conversion material synthesized above:

[0044] (1) figure 1 N of MIP respectively 2 Adsorption-desorption isotherm curve (a) and pore size distribution diagram (b), according to the type of adsorption-desorption curve, the pore characteristics of the sample can be judged. figure 1 (a) It can be seen that N 2 The adsorption-desorption isotherm curve is a typical Langmuir type IV curve, when P / P 0 When greater than 0.4, a wider hysteresis loop appears, indicating that the MIP surface channels have narrower orifices. In addition, the specific surface area of ​​MIP is 38.123m 2 / g, the pore volume is 0.033cm 3 / g. Depend on figure 1 (b) It can be seen that the pore size distribution of MIP is broad and mainly concentrated in the range of 2-50 nm, and the average pore size of mesopores is 3.786 nm. The large specific surface area and moderate pore size of MIP improve the delive...

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Abstract

The invention discloses preparation and application of a perfluorooctane sulfonic acid mesoporous molecularly imprinted fluorescent probe based on an up-conversion material. The method comprises the following steps: by taking amino-modified NaYF4: Yb, Er as a core, N, O-bistrifluoroacetamide as a functional monomer, hexadecyl trimethyl ammonium bromide as a pore-foaming agent, perfluorooctane sulfonic acid as a template molecule and tetraethoxysilane as a cross-linking agent, forming a silicon dioxide thin layer with a specific recognition site for perfluorooctane sulfonic acid on the surface of amino-modified NaYF4: Yb, Er under the initiation of an alkaline condition, and removing the template and the pore-foaming agent to obtain a mesoporous molecularly imprinted fluorescent probe material, wherein the mesoporous molecularly imprinted fluorescent probe material has a good effect when being applied to detection of perfluorooctane sulfonic acid in water. According to the invention, a fluorescence detection technology and a surface molecular imprinting technology are combined, so that the prepared up-conversion molecularly imprinted fluorescent probe has relatively high detection sensitivity and selectivity, the preparation method is scientific and simple to operate, and reaction conditions are easy to control; and the prepared material is green and has a good application prospect.

Description

technical field [0001] The invention relates to the technical field of molecularly imprinted fluorescent probes, in particular to the preparation and application of a perfluorooctane sulfonic acid mesoporous molecularly imprinted fluorescent probe based on an upconversion material. [0002] technical background [0003] Since the 1950s, perfluorooctane sulfonic acid (PFOS) has been widely produced worldwide and used as a raw material for textiles, lubricants, cosmetics, waterproofing materials, and fire-fighting foams due to its hydrophobic and oleophobic properties. Due to the high bond energy (about 110kcal / mol) of the C-F bond in the PFOS structure, it has high thermal stability and chemical inertness in the environment. It is difficult to be decomposed in strong acid, strong alkali and oxidizing agent, and will not undergo photolysis, hydrolysis and biodegradation. Therefore, once PFOS is discharged into the environment, it is difficult to be decomposed. As a ubiquitous ...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/02G01N21/64
CPCC09K11/7773C09K11/025G01N21/643G01N2021/6432G01N2021/6417
Inventor 李晶郭会琴颜流水李可心田凌溪于慧林立钶
Owner NANCHANG HANGKONG UNIVERSITY
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