Preparation method of bisphenol A hapten and bisphenol A complete antigen

A complete antigen and hapten technology, applied in the preparation of organic compounds, carboxylate salts, chemical instruments and methods, etc., can solve the cumbersome preparation of bisphenol A hapten and complete antigen, low product purity, complicated operation, etc. problems, to achieve the effect of short synthesis time, high product purity and broad application prospects

Active Publication Date: 2018-03-27
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the synthesis methods of bisphenol A hapten need to be time-consuming, and the operation is more complicated. high energy consumption

Method used

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  • Preparation method of bisphenol A hapten and bisphenol A complete antigen
  • Preparation method of bisphenol A hapten and bisphenol A complete antigen
  • Preparation method of bisphenol A hapten and bisphenol A complete antigen

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1 1

[0062] Experimental example 1 Sodium monochloroacetate Na 2 CO 3 Methods Synthesis of Bisphenol A Hapten

[0063] Weigh 640 mg of sodium monochloroacetate powder and dissolve it in 4 mL of water to obtain solution A; weigh 270 mg of anhydrous sodium carbonate and dissolve it in 2 mL of water to obtain solution B; weigh 1140 mg of bisphenol A particles and dissolve it in 40 mL of dioxane to obtain Solution C: first add solution A dropwise to solution C, then add solution B dropwise to the mixed solution of A and C, and stir for 9 hours in a water bath at 70°C. Remove the insoluble matter by filtration, evaporate the filtrate under reduced pressure to remove the solvent, suspend the remaining residue in 10mL distilled water, adjust the pH to 3.6 with 6mol / L HCl solution, filter the precipitate, dissolve it in an appropriate amount of boiling chloroform, and add a small amount of petroleum ether , a white precipitate was formed, which was filtered and dried.

[0064] The UV sc...

experiment example 2

[0065] Experimental example 2 Ethyl bromobutyrate K 2 CO 3 (Method 1) Synthesis of bisphenol A hapten

[0066] Weigh 1.14g (5mmol) BPA and 828mg (6mmol) anhydrous K 2 CO 3 Dissolve in 20 mL of anhydrous acetone, add 716 μL of ethyl bromobutyrate, heat the mixture to 70 ° C, and stir under reflux for 8 h. The reaction was cooled and dried by rotary evaporation under vacuum. Mix 10 mL of methanol and 5 mL of 10% NaOH solution, dissolve the solid residue after rotary evaporation and drying in the above mixed solution, and reflux for 30 min under heating. Adjust to pH=2 with 1:1 HCl solution. Add appropriate amount of ethyl acetate to extract 3 times, collect the ethyl acetate phase, anhydrous Na 2 SO 4 After dehydration, the solvent was removed by rotary evaporation.

[0067] The UV scan results of BPA standard (100μg / mL) and hapten (100μg / mL) figure 2 . Comparing the two curves, it can be seen that both the BPA standard and the BPA hapten have characteristic absorptio...

experiment example 3

[0069] Experimental example 3 Ethyl bromobutyrate K 2 CO 3 (Method 2) Synthesis of bisphenol A hapten

[0070] Weigh 1.004g (4.4mmol) BPA and 1.348g (9.75mmol) anhydrous K 2 CO 3 Dissolve in 10 mL of anhydrous DMF to obtain a mixed solution, add 697 μL (4.87 mmol) ethyl bromobutyrate dropwise to the above mixed solution, and stir overnight at 75° C. under airtight condition. Add 5 mL of 10% NaOH solution, heat for 30 min, and adjust to pH=2 with 1:1 HCl solution. The mixed solution was extracted 3 times with ethyl acetate, 30mL each time, the ethyl acetate phase was collected, and anhydrous Na 2 SO 4 Dehydration treatment, evaporated to dryness under reduced pressure.

[0071] The UV scan results of BPA standard (100μg / mL), DPA standard (100μg / mL) and BPA hapten (100μg / mL) Figure 4 . Comparing the three curves, it can be seen that the BPA standard, DPA standard and BPA hapten all have characteristic absorption peaks at 278nm, and there is no obvious shift in the maxim...

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Abstract

The invention discloses a preparation method of a bisphenol A hapten and a bisphenol A complete antigen. The preparation method comprises the steps of enabling bisphenol A, which is taken as a raw material, to react with monochloroacetate in presence of a catalyst-potassium hydroxide / sodium hydroxide, removing the unreacted bisphenol A by using ethyl acetate, then acidizing by using hydrochloric acid to obtain a product, filtering, washing, and drying to obtain the bisphenol A carboxylated hapten; coupling the bisphenol A hapten with a carrier protein OVA by using a carbodiimide method so as to prepare the bisphenol A complete antigen. The preparation method provided by the invention is simple, convenient and rapid, and greatly shortens the reaction time on the basis of guaranteeing the product purity and yield; furthermore, after the preparation method is adopted, heating and pH control are not needed, so that the industrial production cost is lowered.

Description

technical field [0001] The invention relates to the technical fields of biochemical engineering and food detection, in particular to a method for preparing a bisphenol A hapten and a complete antigen. Background technique [0002] Bisphenol A (Bisphenol A), abbreviated as BPA, scientific name 2,2-bis(4-hydroxyphenyl)propane, referred to as diphenolic propane, molecular formula C 15 h 16 o 2 , the pure product is white crystal, flammable, slightly phenol smell, soluble in acetic acid, ethanol, methanol, isopropanol, butanol, acetone, ether, benzene and alkaline solution, slightly soluble in carbon tetrachloride, hardly Dissolved in water. Bisphenol A is a chemical substance with low toxicity, which can cause moderate irritation to the respiratory tract, skin, cornea and digestive tract. Bisphenol A has the characteristics of mimicking estrogen, which can imitate or interfere with endogenous estrogen. Many studies have proved that it will have a series of adverse effects o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/367C07C59/70C07K14/765C07K14/77C07K14/795C08G69/10
CPCC07C51/367C07C59/70C07K14/765C07K14/77C07K14/795C07K19/00C08G69/10
Inventor 贾敏唐洁刘小帆刘庄琳
Owner SHANDONG NORMAL UNIV
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