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Magnetic core-shell imprinted material of silibinin and preparation method thereof

A technology of silibinin and imprinted materials, applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., can solve problems affecting silybin production, price and application, poor selectivity, waste, etc., to achieve High reusability, easy cleaning, and strong practicability

Active Publication Date: 2020-05-01
NANHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For a long time, people have used traditional extraction and separation techniques (solvent extraction, fractional distillation, steam distillation, adsorption, microwave-assisted extraction, supercritical CO 2 Extraction method, enzyme-assisted extraction method, etc.) to obtain silybin from the medicinal material milk thistle often has disadvantages such as low efficiency, time-consuming, waste material, poor selectivity, etc., which greatly affects the output, price and application of silybin

Method used

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  • Magnetic core-shell imprinted material of silibinin and preparation method thereof
  • Magnetic core-shell imprinted material of silibinin and preparation method thereof
  • Magnetic core-shell imprinted material of silibinin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1: A magnetic core-shell imprinted material that selectively adsorbs silybin, is easy to separate, easy to clean, and has a high reuse rate. The mass percentage of each component of the imprinted material is: silybin 0.220%; Methacrylic acid 0.110%; Ethylene glycol dimethacrylate 1.813%; Fe 3 o 4 &SiO 2 -MPS 0.915%; Pentamethyldiethylenetriamine 0.153%; Copper Bromide 0.091%; Azobisisobutyronitrile 0.549%; Acetonitrile 96.149%;

[0042] Its preparation method is as follows:

[0043] a. Add 0.220% silibinin, 96.149% acetonitrile and 0.110% methacrylic acid MAA to a round bottom flask by mass percentage, and place it in an orbital shaker for 12 hours at room temperature, so that the template molecule silibinin and functional Monomer MMA fully pre-polymerized;

[0044] b. In the above-mentioned pre-polymerization liquid, adding mass percent successively is 1.813% crosslinking agent ethylene glycol dimethacrylate (EMGDA), 0.549% initiator azobisisobutyronitrile ...

Embodiment 2

[0049] Example 2: A magnetic core-shell imprinted material that selectively adsorbs silybin and is easy to separate, easy to clean, and highly reusable. The mass percentage of each component of the imprinted material is: silybin 0.214%; Methacrylic acid 0.191%; Ethylene glycol dimethacrylate 3.527%; Fe 3 o 4 &SiO 2 -MPS 1.780%; Pentamethyldiethylenetriamine 0.148%; Copper bromide 0.089%; Azobisisobutyronitrile 0.534%; Acetonitrile 93.514%;

[0050] Its preparation method is as follows:

[0051] a. Add 0.214% silibinin, 93.514% acetonitrile and 0.191% methacrylic acid MAA in a round bottom flask by mass percentage, and place it in an orbital shaker for 12 hours at room temperature, so that the template molecule silibinin and functional Monomer MMA fully pre-polymerized;

[0052] b. In the above-mentioned pre-polymerization solution, adding mass percent successively is 3.527% crosslinking agent ethylene glycol dimethacrylate (EMGDA), 0.534% initiator azobisisobutyronitrile (...

Embodiment 3

[0057] Example 3: A magnetic core-shell imprinted material with selective adsorption on silybin, convenient separation, easy cleaning, and high reusability. The mass percentage of each component required to prepare the imprinted material is: water Silybin 0.209%; Methacrylic acid 0.261%; Ethylene glycol dimethacrylate 5.150%; Fe 3 o 4 &SiO 2 -MPS2.599%; pentamethyldiethylenetriamine 0.145%; copper bromide 0.087%; azobisisobutyronitrile 0.520%; acetonitrile 91.035%;

[0058] Its preparation method is as follows:

[0059] a. Add 0.209% silibinin, 91.035% acetonitrile and 0.261% methacrylic acid MAA in a round bottom flask by mass percentage, place it in an orbital shaker for 12 hours at room temperature, so that the template molecule silibinin and functional Monomer MMA fully pre-polymerized;

[0060] b. In the above-mentioned pre-polymerization solution, adding mass percent successively is 5.150% crosslinking agent ethylene glycol dimethacrylate (EMGDA), 0.520% initiator az...

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Abstract

The invention relates to a silibinin magnetic core-shell type imprinting material and a preparation method thereof. The preparation method comprises the following steps: putting template molecules, namely silibinin, a monomer, namely, methacrylic acid and a pore forming agent, namely acetonitrile, into a reaction container, implementing a reaction, after a pre-reaction, respectively putting a cross-linking agent, namely ethylene glycol dimethacrylate, an initiator, namely azodiisobutyronitrile, a magnetic core, namely Fe3O4&SiO2-<MPS, catalysts, namely pentamethyl diethylenetriamine and cupricbromide, introducing nitrogen, performing reactions in the presence of nitrogen, thoroughly drying an obtained surface imprinting polymer in a drying oven of 60 DEG C, repeatedly eluting, removing residual acetic acid in the material with ethanol, performing vacuum drying on the eluted imprinting material, and performing material discharge. By adopting the method, multiple defects that a conventional extraction separation technique is low in efficiency, serious in material waste, long in time, poor in specificity and the like in the field of natural products, are overcome, and in addition, the target imprinting material is good in selective adsorption upon silibinin, convenient to separate, simple and easy to clean and high in recycling rate.

Description

technical field [0001] The invention relates to the technical field of magnetic molecular imprinting, in particular to a silibinin magnetic core-shell imprinting material and a preparation method thereof. Background technique [0002] Active ingredients in natural products generally have many characteristics such as complex structure, diverse ingredients, low content, and unstable properties, so it is often very difficult to separate pure effective active ingredients from natural medicinal materials. In the past, traditional separation methods such as filtration and centrifugation can only obtain crude extracts, but it is difficult to obtain a single pure component. However, modern separation techniques such as chromatography, ultrafiltration, and adsorption methods generally have specific selectivity for the analyzed object. Low, poor affinity and other disadvantages, and the solvent used in the above conventional separation method consumes a lot, the efficiency is low, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/14C08F220/06C08F2/44C08K3/22C08K3/36C08J9/28B01J20/26B01J20/28C08L35/02
CPCB01J20/268B01J20/28021C08F2/44C08F222/14C08J9/0066C08J9/28C08J2335/02C08K3/22C08K3/36C08K2003/2275C08F220/06
Inventor 谭倪高阳林英武何典雄蒋敏王娟韩敬文季康
Owner NANHUA UNIV
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