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A imprinted material with high recognition ability for icariin and its preparation method

An imprinting material, icariin technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of inability to purify with trace substances, poor selectivity, time-consuming, etc., and achieves simple operation, high affinity, good economic effect

Inactive Publication Date: 2016-10-05
NANHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For a long time, using traditional separation techniques (solvent extraction, fractionation, steam distillation, adsorption, etc.) The reported modern extraction and separation technologies mainly include: ultrasonic technology, macroporous adsorption resin technology, ultrafiltration technology, enzyme engineering technology, microwave extraction technology, semi-bionic extraction method, ionic liquid extraction, supercritical fluid extraction technology, high-speed countercurrent chromatographic separation, etc. Although these techniques have improved the extraction efficiency of icariin to a certain extent, their selectivity is poor and cannot be used for the purification of trace substances

Method used

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  • A imprinted material with high recognition ability for icariin and its preparation method
  • A imprinted material with high recognition ability for icariin and its preparation method
  • A imprinted material with high recognition ability for icariin and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: An imprinted material (MIPs) with a high ability to recognize icariin. The mass percentages of the components required to prepare the imprinted material are: 0.10% icariin, 0.02% acrylamide, 1.22% Ethylene glycol dimethacrylate, 0.10% azobisethylbutyronitrile and 98.56% methanol-acetonitrile mixed solvent.

[0035] The mixed solvent is a mixed solution of methanol and acetonitrile in a volume ratio of 3:1.

[0036] Its preparation method is as follows:

[0037] A. Add 0.10% icariin, 0.02% acrylamide and 98.56% methanol-acetonitrile mixed solvent in the reaction kettle by mass percentage, stir at room temperature for 6 hours, and then let stand for 1 hour to make it fully pre-polymerized;

[0038] The volume ratio of the methanol-acetonitrile mixed solution is 3:1;

[0039] B. After pre-polymerization, add 1.22% ethylene glycol dimethacrylate and 0.10% azobisethylbutyronitrile respectively by mass percentage, ultrasonically degas for 15 minutes, then fill wi...

Embodiment 2

[0043] Example 2: An imprinted material (MIPs) with a high ability to recognize icariin. The mass percentages of the components required to prepare the imprinted material are: 0.10% icariin, 0.11% acrylamide, 1.22% Ethylene glycol dimethacrylate, 0.10% azobisethylbutyronitrile and 98.47% methanol-acetonitrile mixed solvent.

[0044] The mixed solvent is a mixed solution of methanol and acetonitrile in a volume ratio of 3:1.

[0045] Its preparation method is as follows:

[0046]A. Add 0.10% icariin, 0.11% acrylamide and 98.47% methanol-acetonitrile mixed solvent in the reaction kettle by mass percentage, stir at room temperature for 6 hours, and then let stand for 1 hour to make it fully pre-polymerized;

[0047] The volume ratio of the methanol-acetonitrile mixed solution is 3:1;

[0048] B. After pre-polymerization, add 1.22% ethylene glycol dimethacrylate and 0.10% azobisethylbutyronitrile respectively by mass percentage, ultrasonically degas for 15 minutes, then fill wit...

Embodiment 3

[0052] Example 3: An imprinted material (MIPs) with a high ability to recognize icariin. The mass percentages of the components required to prepare the imprinted material are: 0.10% icariin, 0.06% acrylamide, 2.99% Ethylene glycol dimethacrylate, 0.10% azobisethylbutyronitrile and 96.75% methanol-acetonitrile mixed solvent.

[0053] The mixed solvent is a mixed solution of methanol and acetonitrile in a volume ratio of 3:1.

[0054] Its preparation method is as follows:

[0055] A. Add 0.10% icariin, 0.06% acrylamide and 96.75% methanol-acetonitrile mixed solvent in the reaction kettle by mass percentage, stir at room temperature for 6 hours, and then let stand for 1 hour to make it fully pre-polymerized;

[0056] The volume ratio of the methanol-acetonitrile mixed solution is 3:1;

[0057] B. After pre-polymerization, add 2.99% ethylene glycol dimethacrylate and 0.10% azobisethylbutyronitrile respectively by mass percentage, ultrasonically degas for 15 minutes, then fill wi...

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Abstract

The invention relates to an imprinting material with high capacity of recognizing icariin and a preparation method of the imprinting the material. The preparation method comprises the following steps of: adding the icariin, acrylamide and a mixed solvent into a reactor, stirring for 6 hours at room temperature, and standing for 1 hour for thorough pre-polymerization to obtain a pre-polymerized liquid mixture; adding ethylene glycol dimethacrylate and azobisisobutyronitrile into the pre-polymerized liquid mixture, degassing the mixture for 15 minutes with ultrasonic waves, introducing nitrogen into the pre-polymerized liquid mixture for 30 minutes, sealing, and putting in a water bath of 70 DEG C for thermostatic reaction of 24 hours to obtain an imprinting polymer; diluting the prepared imprinting polymer with the mixed solution of methanol and acetic acid at a volume ratio of 7: 3 until no icariin (template molecule) can be detected in an eluate; washing away the redundant acetic acid by the methanol, and finally the drying the diluted imprinting polymer for 24 hours in vacuum at the temperature of 60 DEG C to obtain the imprinting material. The imprinting material provided by the invention is high compatible to the icariin. The defects of low efficiency, time consumption and material waste of the traditional separation technology which is used for separating the icariin from epimedium are overcome.

Description

technical field [0001] The invention relates to the technical field of molecular imprinting, which is a method of forming a complex through a non-covalent bond between a template molecule and a functional monomer in a suitable solvent, and then adding a cross-linking agent and an initiator to cause a polymerization reaction to occur, and then from the generated The imprinted material with three-dimensional holes that is completely complementary to the size, shape, and functional groups of the template molecule can be obtained by removing the template molecule from the polymer. This material can be applied to solid-liquid phase extraction and separation. Background technique [0002] The extraction and separation of active ingredients in natural medicines has always been an important and difficult point in the research of natural medicinal chemistry. [0003] Epimedium is a plant of the genus Epimedium in the Berberidaceae family. It is one of the Chinese herbal medicines wit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/14C08F220/56C08J9/26B01J20/26B01J20/30
Inventor 谭倪贾晓鹤程易颜雪明张稳廖森侯丹杨雪纯
Owner NANHUA UNIV
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