Functional material for adsorbing trace histamine and preparation method and application of functional material

A functional material, histamine technology, applied in the selection of adsorption, chemical instruments and methods, and material absorption and weighing, etc., can solve the problems of uneven particle size, low mass transfer speed, poor rigidity, etc., to achieve uniform particle size, The effect of improving dispersibility and high selection specificity

Active Publication Date: 2013-01-30
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a highly selective adsorption method for histamine that combines with sol-gel technology in order to overcome the defects of low mass transfer rate, uneven particle size and poor rigidity of traditional molecularly imprinted polymers. Materials and their preparation methods and applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for preparing a functional material that absorbs trace amounts of histamine, the steps of the preparation method are:

[0022] (1) Add 0.9mmol histamine to 170mmol methanol solvent, add 4.5mmol 3-mercaptopropyltriethoxysilane after it is completely dissolved, stir in a water bath at 55°C for 30min, then add 2.25mmol tetraethoxysilane for the same Under the condition of reaction for 30min, then add 0.1mol / L ammonia water 0.25mmol and place in a round bottom flask, incubate at 55°C for 14h;

[0023] (2) Filter 5 g of the above-mentioned polymerized product through methanol and age at 60°C for 10 hours, then add 100 mL of hydrochloric acid and methanol solution with a mass ratio of 1:85.58, stir for 4 hours, and filter with 1 mol / L Wash with sodium hydroxide and secondary deionized water until neutral;

[0024] (3) Extract 300 mL of the prepared powdery polymer with methanol: glacial acetic acid at a volume ratio of 9:1 in a Soxhlet extractor for 16 hours; vacuum...

Embodiment 2

[0027] Applications of the above materials in piezoelectric quartz microbalance sensors:

[0028] Dissolve 9.69 mg of polyvinyl chloride in 1 mL of dichloromethane, disperse the invented powdery histamine adsorption material in it, take 5 μL and evenly hang it on a quartz wafer, and dry it in vacuum at 35°C for 12 hours. The prepared histamine piezoelectric quartz microbalance sensor is used to detect histamine in food, and the detection limit can reach 2.57nmol / L.

Embodiment 3

[0030] Application of the above-mentioned materials in the detection of histamine by solid phase extraction-high performance liquid chromatography:

[0031] Accurately weigh 50mg of the invented powdered histamine adsorption material and put it in a solid phase extraction column (3.0cm×1.0cmi.d.) for the purification and enrichment of histamine in the sample extract, combined with high performance liquid chromatography Analytical technology detects histamine in food, and the detection limit can reach 9nmol / L.

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Abstract

The invention discloses a functional material for adsorbing trace histamine and a preparation method for the functional material and application of the functional material. The functional material is synthesized by taking histamine as template molecules, 3-mercaptopropyltriethoxy-silane as a functional monomer, tetraethoxysilane as a crosslinking agent and methanol as a pore-foaming agent by utilizing a sol-gel technology and a molecular imprinting technique, wherein the adsorption capacity of the functional material is 12.758mg / g. The functional material has high physical and chemical stability and can resist high temperature, high pressure, acid-base, organic solvents and the like and is low in cost and simple in synthetic process, the reaction conditions are easy to control, the prepared histamine specificity adsorbing material can be used for electrochemical electrode modification and combined solid-phase extraction enrichment and high performance liquid chromatography and is suitable for detection of trace histamine in animal derived foods.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a specific selective adsorption material for trace histamine, its preparation method and application. Background technique [0002] The chemical name of histamine (Histamine, HA) is 4(5)-(2-aminoethyl)imidazole. Substances with the greatest health impact. HA is generally readily metabolized and well tolerated in food. However, if the concentration of HA in food exceeds the normal level due to bacterial contamination, it will cause harm to the body. HA poisoning is one of the main safety problems in aquatic food. In recent years, HA poisoning incidents have occurred frequently all over the country, especially in coastal areas. HA can cause a series of allergic reactions such as headache, itchy rash, hypotension, etc. It has a strong stimulating effect on the digestive tract and can cause gastrointestinal bleeding and erosion. Its residues in animal-derived foods direc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30B01D15/08G01N5/02
Inventor 张燕王硕王俊平戴洁
Owner TIANJIN UNIV OF SCI & TECH
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