A surface imprinted material selectively adsorbing nordihydroguaiaretic acid and its preparation method

A technology of dihydroguaiaretic acid and surface imprinting, applied in chemical instruments and methods, and other chemical processes, can solve the problems of poor practicability, poor selectivity, and low yield, and achieve high reuse rate and easy cleaning , the effect of high affinity

Inactive Publication Date: 2017-06-30
NANHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the extraction and separation of NDGA, there are mainly reports at home and abroad on organic solvent extraction, ultrasonic extraction, and high-performance liquid chromatography separation. Although these technologies have improved the extraction efficiency of nordihydroguaiaretic acid to a certain extent, their Poor selectivity, low output, poor practicability

Method used

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  • A surface imprinted material selectively adsorbing nordihydroguaiaretic acid and its preparation method
  • A surface imprinted material selectively adsorbing nordihydroguaiaretic acid and its preparation method
  • A surface imprinted material selectively adsorbing nordihydroguaiaretic acid and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: A surface imprinted material that selectively adsorbs nordihydroguaiaretic acid, is easy to clean, and has good application performance. The mass percentage of each component required to prepare the imprinted material is: nordihydroguaiaretic acid Acetate 0.222%; γ-Aminopropyltriethoxysilane 0.819%; Methyltriethoxysilane 0.264%; Tetraethyl orthosilicate 12.335%; Silicon dioxide 1.480%; 0.01mol L -1 Acetic acid solution 14.803%; porogen ethanol 70.076%.

[0034] Its preparation method is as follows:

[0035]A. Add 0.222% nordihydroguaiaretic acid, 0.819% γ-aminopropyltriethoxysilane, 0.264% methyltriethoxysilane and 70.076% porogen ethanol to the reaction kettle by mass percentage , stirred at room temperature for 1 hour to make it fully pre-reacted;

[0036] B. After the pre-reaction, add 1.480% silicon dioxide and 12.335% tetraethyl orthosilicate respectively by mass percentage, stir at room temperature for 1 hour, and then add 14.803% with a concentration...

Embodiment 2

[0041] Example 2: A surface imprinted material with selective adsorption to nordihydroguaiaretic acid, easy to clean, and good application performance. The mass percentage of each component required to prepare the imprinted material is: nordihydroguaiaretic acid Acetate 0.212%; γ-Aminopropyltriethoxysilane 0.939%; Methyltriethoxysilane 0.252%; Tetraethyl orthosilicate 14.732%; Silicon dioxide 2.827%; 0.01mol L -1 Acetic acid solution 14.134%; porogen ethanol 66.913%.

[0042] Its preparation method is as follows:

[0043] A. Add 0.212% nordihydroguaiaretic acid, 0.939% γ-aminopropyltriethoxysilane, 0.252% methyltriethoxysilane and 66.913% porogen ethanol to the reaction kettle by mass percentage , stirred at room temperature for 1 hour to make it fully pre-reacted;

[0044] B. After the pre-reaction, add 2.827% silicon dioxide and 14.732% tetraethyl orthosilicate respectively by mass percentage, stir at room temperature for 1 hour, and then add 14.134% with a concentration o...

Embodiment 3

[0049] Example 3: A surface imprinted material that selectively adsorbs nordihydroguaiaretic acid, is easy to clean, and has good application performance. The mass percentage of each component required to prepare the imprinted material is: nordihydroguaiaretic acid Acetate 0.203%; γ-Aminopropyltriethoxysilane 1.048%; Methyltriethoxysilane 0.241%; Tetraethyl orthosilicate 16.905%; Silicon dioxide 4.057%; 0.01mol L -1 Acetic acid solution 13.524%; porogen ethanol 64.022%.

[0050] Its preparation method is as follows:

[0051] A. Add 0.203% nordihydroguaiaretic acid, 1.048% γ-aminopropyltriethoxysilane, 0.241% methyltriethoxysilane and 64.022% porogen ethanol to the reaction kettle by mass percentage , stirred at room temperature for 1 hour to make it fully pre-reacted;

[0052] B. After the pre-reaction, add 4.057% silicon dioxide and 16.905% tetraethyl orthosilicate respectively by mass percentage, stir at room temperature for 1 hour, and then add 13.524% with a concentratio...

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Abstract

The invention relates to a surface imprinted material capable of selectively adsorbing nordihydroguaiaretic acid and a preparation method thereof. The preparation method comprises the following steps: adding nordihydroguaiaretic acid, gamma-aminopropyltriethoxysilane, methyltriethoxysilane and a pore-forming agent ethanol into a reaction kettle, stirring at room temperature for 1 hour to perform sufficient pre-reaction; after the pre-reaction, respectively adding silicon dioxide and tetraethyl orthosilicate into the prepolymer solution, stirring at room temperature for 1 hour, adding a right amount of 0.01 mol L<-1> acetic acid solution, and stirring at room temperature to react for 24 hours, thereby obtaining a surface imprinted polymer; and adding 0.2g of dried surface imprinted polymer into a 50mL Soxhlet extraction device, eluting with a mixed solution of ethanol and acetic acid in a volume ratio of 7:3 for 8 hours until no nordihydroguaiaretic acid can be detected in the eluate, washing the material with ethanol to remove the residual acetic acid, carrying out vacuum drying on the eluted imprinted polymer at 60 DEG C for 24 hours, and discharging. The material has favorable adsorption selectivity for nordihydroguaiaretic acid, is simple to clean and high in applicability, and overcomes the defects of low efficiency, material consuming, time consuming and the like in the traditional separation technique.

Description

technical field [0001] The present invention relates to the technical field of surface molecular imprinting, which is a method of forming a complex through non-covalent bond interaction between template molecules and functional monomers in a suitable solvent, and then adding a carrier and a cross-linking agent, under the action of an initiator, Specific imprinting sites are formed on the surface of the carrier. After removing the template molecules, a surface imprinting material that is completely complementary to the size, shape, and functional groups of the template molecules and has three-dimensional holes can be obtained on the surface of the carrier. This material can be applied to the extraction of related template molecules and separation, and easy to clean, good application performance. Background technique [0002] The active ingredients of natural products often have many characteristics such as complex structure, diverse ingredients, low content and unstable prope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/26C08K3/36C08J9/26B01J20/26B01J20/30
Inventor 谭倪廖森侯丹杨雪纯张稳贾晓鹤
Owner NANHUA UNIV
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