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Preparation method of bisphenol A magnetic molecularly imprinted polymer and application of bisphenol A magnetic molecularly imprinted polymer in bisphenol A fluorescence detection

A magnetic molecular imprinting and polymer technology, which is applied in the field of analytical chemistry, can solve problems such as limitations, affecting the accuracy of results, and changes in fluorescent signals, and achieve the effects of easy operation, cheap reagents, and low sensitivity improvement

Active Publication Date: 2021-03-26
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, certain matrix backgrounds in food will cause changes in the fluorescent signal, thereby affecting the accuracy of the results, so the application of this method in food is often limited by the sample pretreatment method

Method used

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  • Preparation method of bisphenol A magnetic molecularly imprinted polymer and application of bisphenol A magnetic molecularly imprinted polymer in bisphenol A fluorescence detection
  • Preparation method of bisphenol A magnetic molecularly imprinted polymer and application of bisphenol A magnetic molecularly imprinted polymer in bisphenol A fluorescence detection
  • Preparation method of bisphenol A magnetic molecularly imprinted polymer and application of bisphenol A magnetic molecularly imprinted polymer in bisphenol A fluorescence detection

Examples

Experimental program
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Effect test

Embodiment 1

[0044] A method for preparing a bisphenol A magnetic molecularly imprinted polymer, comprising the following steps:

[0045] Step 1: Mix 0.0428g of bisphenol A (BPA), 775μL of 4-VP, and 90mL of anhydrous acetonitrile, stir evenly in an ice bath and nitrogen protection, and store in a refrigerator at 4°C overnight after the reaction . Add 0.3g Fe to the mixture 3 o 4 @SiO 2 , 9mL of TRIM, 90mL concentration is 167mg mL -1 The AIBN acetonitrile solution was first reacted at 50°C for 6h under nitrogen protection, and then reacted at 60°C for 24h. Separate the product by applying an external magnetic field and wash and dry it for use;

[0046] Step 2: Soxhlet extraction of the material obtained in Step 4 with methanol-acetic acid mixed solution (9:1, v / v) for 30 hours, and vacuum-drying the washed product to obtain bisphenol A magnetic molecularly imprinted polymers (BMMIPs 1 ). In addition to not adding the template molecule bisphenol A, the corresponding non-imprinted pol...

Embodiment 2

[0058] A magnetic molecularly imprinted polymer tandem fluorescence analysis involved in this example is used for the detection of bisphenol A, including the following steps:

[0059] Weigh 5mg of the bisphenol A imprinting material prepared in Example 1, add to 5mL of spiked 30ng mL -1 , 50ng mL -1 , 80ngmL -1 In the actual sample of tap water, oscillate on a shaking table at room temperature for 5 minutes. After the adsorption is complete, separate it with a magnet, pour off the supernatant, add 1 mL of anhydrous methanol to the bisphenol A imprinted material, and ultrasonically elute. Repeat three times, and wash After deliquoring and merging, blow dry with nitrogen, add ultrapure water, vortex for a few seconds, and mix well, then add 2.7×10 -5 mol L -1 Acridine orange solution 2mL, 5.0×10 -3 mol L -1 h 2 SO 4 Solution 80 μL, 1.0×10 -3 mol L -1 FeSO 4 Solution 0.6mL, 2×10 -3 mol L -1 H 2 o 2 Solution 1mL, dilute to 10mL with ultrapure water, shake well, place...

Embodiment 3

[0061] A method for detecting magnetic molecularly imprinted polymers and fluorescently bound bisphenol A involved in this embodiment includes the following steps:

[0062] Weigh 5 mg of the bisphenol A imprinting material prepared in Example 1, and add it to the 5 mL of the standard spiked 30 ng mL -1 , 50ng mL -1 , 80ng mL -1 In the actual sample of orange juice, shake the shaker at room temperature for 5 minutes after the adsorption is complete, separate with a magnet, pour off the supernatant, add 1mL of anhydrous methanol to the bisphenol A imprinted material, and ultrasonically elute, repeat three times, and eluate After merging, blow dry with nitrogen, add ultrapure water, vortex, and mix well, then add 2.7×10 -5 mol L -1 Acridine orange solution 2mL, 5.0×10 -3 mol L -1 h 2 SO 4 Solution 80 μL, 1.0×10 -3 mol L -1 FeSO 4 Solution 0.6mL, 2×10 -3 mol L -1 H 2 o 2 Solution 1mL, dilute to the mark with ultrapure water, shake well, place in 45°C constant tempera...

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Abstract

The invention discloses a preparation method of a bisphenol A magnetic molecularly imprinted polymer and application of the bisphenol A magnetic molecularly imprinted polymer in bisphenol A fluorescence detection, and belongs to the field of analytical chemistry. The preparation method comprises the steps of modifying the surfaces of Fe3O4 nanoparticles, synthesizing Fe3O4@SiO2 nanoparticles through a sol-gel method on the basis, and carrying out double bond modification by using MPS to obtain the ideal magnetic core vinyl-Fe3O4@SiO2; further polymerizing with template molecules bisphenol A, 4-VP, TRIM and AIBN in an acetonitrile solution to form the BMMIPs with a novel core-shell structure; and applying the obtained BMMIPs to sample pretreatment, and establishing a rapid enrichment, separation and detection method of bisphenol A in a liquid food sample in combination of fluorescence reaction of acridine orange and bisphenol A. The method has the advantages of simple operation, stronganti-interference capability, high sensitivity, short time consumption and the like. According to the method, standard recovery is carried out on actual samples (ultrapure water, mineral water, orangejuice and the like), the recovery rate is 85.4%-88.7%, the relative standard deviation is less than 7.2%, and the sample detection limit is 16.5[mu]g L<-1>.

Description

technical field [0001] The invention relates to the synthesis of a magnetic molecular imprinted nanomaterial with specific enrichment of bisphenol A, and the application of the material to the fluorescence detection of bisphenol A in a liquid food medium. The establishment of the method can achieve the purpose of specific enrichment and rapid separation and detection of bisphenol A in complex food samples, and belongs to the field of analytical chemistry. Background technique [0002] Bisphenol A is an environmental estrogen with strong biological toxicity and endocrine disrupting effect. It is widely used in food-grade packaging materials and plastic products. It can be transmitted through the food chain, enter the human body and produce accumulation, and interfere with the human endocrine system. , the resulting agricultural products and food safety issues have received widespread attention. [0003] At present, there are two major problems in the monitoring of pollutants...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F226/06C08F222/14C08J9/26G01N21/64G01N30/02G01N30/06B01J20/26B01J20/30B01J20/28
CPCC08F292/00C08J9/26G01N21/64G01N30/02G01N30/06B01J20/268B01J20/264B01J20/28009C08J2201/0422C08J2351/10G01N2030/062B01J2220/4812B01J2220/4806C08F226/06
Inventor 卢一辰张佳凤熊晓辉李婷婷肖维玮毛佳昊陈昊东郑彬洪鸿亮
Owner NANJING UNIV OF TECH
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