Bisphenol A dummy template molecular imprinting stirring rod of and preparation method thereof

A technique of molecular imprinting and pseudo-template, applied in chemical instruments and methods, preparation of test samples, and other chemical processes, can solve problems such as template leakage, residual coating template molecules, and inaccurate measurement results, and achieve high Effects of selectivity, simplicity of materials, and simplicity of the alkylation process

Inactive Publication Date: 2012-07-04
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if the target molecule bisphenol A is used as the template molecule, even after multiple elutions, there will still be template molecules remaining in the coating, which will cause "template leakage" during the sample measurement process, resulting in inaccurate measurement results. precise

Method used

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  • Bisphenol A dummy template molecular imprinting stirring rod of and preparation method thereof
  • Bisphenol A dummy template molecular imprinting stirring rod of and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for preparing a bisphenol A pseudo-template molecularly imprinted stirring bar, comprising the following steps:

[0035] 1) Put an iron core in a glass rod (30mm×5mm i.d.), and sinter both ends ( figure 1 shown in A). The glass rod was successively treated with 1mol L before the alkylation treatment -1 NaOH solution and 0.1mol L -1 Soak in hydrochloric acid solution for 6 hours, then fully rinse with distilled water, and finally, place the activated glass rod in a vacuum drying oven, dry it at 120°C for 1 hour, and set it aside.

[0036] 2) Soak the glass rod treated in step 1) in an acetone solution of 10% (v / v) 3-(methacryloyloxy)propyltrimethoxysilane for 2 hours, rinse with methanol, and blow dry with nitrogen, as a coated carrier.

[0037] 3) Preparation of pre-polymerization solution: In 3 mL of methanol, sequentially add 1 mmol of tetrabromobisphenol A, 2 mmol of tetravinylpyridine, 4 mmol of ethylene glycol dimethacrylate and 30 mg of azobisisobutyr...

Embodiment 2

[0040] Embodiment 2 Adsorption experiment control example

[0041] The commercially available non-molecularly imprinted stirring rod --- PDMS stirring rod (purchased from Dexiang Technology Co., Ltd.), and the bisphenol A pseudo-template molecularly imprinted stirring rod prepared in Example 1 were respectively subjected to adsorption tests under the same conditions. Conditions: Dilute 6mL of milk to 30mL, and adjust the pH to 6-7. Put a stirring rod in the solution, and adsorb at 300 rpm for 1 to 2 hours under the condition of 20°C to 25°C. After the adsorption is complete, use 1 mL of methanol to desorb the stirring rod. After the desorption liquid nitrogen was blown dry, it was reconstituted with 150 μL methanol, and the reconstituted solution was used for liquid phase detection.

[0042] The result is as figure 2 As shown, before extraction, the chromatographic peak of bisphenol A cannot be seen in the chromatogram of milk (shown in chromatographic curve B). After the...

Embodiment 3

[0044] Preparation method of bisphenol A pseudo-template molecularly imprinted stirring rod, glass rod activation using 0.5mol L -1NaOH solution and 0.05mol L -1 Soak the hydrochloric acid solution for 10 hours; soak the glass rod in the acetone solution of 15% by volume of 3-(methacryloyloxy)propyltrimethoxysilane for 4 hours, the quality of azobisisobutyronitrile is tetrabromobisphenol A, tetravinylpyridine , 3% of the mass sum of ethylene glycol dimethacrylate. All the other are the same as in Example 1.

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PUM

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Abstract

The invention relates to a bisphenol A dummy template molecular imprinting stirring rod of and a preparation method thereof, which is characterized in that an alkylated glass rod is used as a carrier, composite macromolecule coating is coated so as to obtain the stirring rod, and the macromolecule coating is bisphenol A dummy template molecular imprinted polymer. The composite process of the bisphenol A dummy template molecular imprinted polymer on the glass rod is as follows: the surface of the glass rod, on which silanol is exposed, is treated by silanization, then reacts with tetrabromobisphenol A, tetra-vinylpyridine, ethylene glycol dimethacrylate and azobisisobutyronitrile, and then the dummy template molecule tetrabromobisphenol A is eluted so as to obtain the bisphenol A dummy template imprinted polymer. The bisphenol A dummy template molecular imprinting stirring rod obtained by the invention is high in specific selectivity of bisphenol A, is good in interference resisting capacity, is high in sensitivity, is free from template leakage problem, and is high in the measurement accuracy of trace bisphenol A in water-bearing medium.

Description

technical field [0001] The invention relates to a method for preparing a bisphenol A pseudo-template molecularly imprinted stirring rod, and the stirring rod can be used for selectively separating and enriching bisphenol A in an aqueous solution. Background technique [0002] Stir Bar Sorptive Extraction (SBSE) is a new type of sample pretreatment method, which was proposed by Erik Baltussen et al. in 1999. It is developed from Solid Phase Microextraction (SPME), and inherits the advantages of Solid Phase Microextraction, integrating extraction, concentration and desorption. However, the volume of the extraction stationary phase is more than 50 times larger than that of the Fiber-SPME extraction stationary phase, and the adsorption surface area is large, so it has higher extraction capacity and sensitivity than solid-phase microextraction. In addition, the stirring bar completes the adsorption of the analyte while stirring itself, avoiding the competitive adsorption of the ...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30G01N1/34G01N1/40
Inventor 胡琴湛雯魏芳弟许贯虹蔡政杨静
Owner NANJING MEDICAL UNIV
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