Preparation method and application of molecularly imprinted membrane for separation of phenylethanoid glycosides

A technology of molecularly imprinted membrane and phenylethanol glycosides, which is applied in the fields of semipermeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve the problems of few types of materials, low product purity, easy membrane pollution, etc., and achieve simple preparation process, The effect of low energy consumption and easy operation

Inactive Publication Date: 2020-03-06
SHIHEZI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Membrane separation method can highly enrich the active ingredients of natural products, reduce impurities, and improve the purity of products efficiently. It has the advantages of mild operating conditions, high selectivity, and low energy consumption. There are disadvantages such as few types of materials, easy contamination of the membrane, and low product purity, which limit its application

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0021] A method for preparing a molecularly imprinted membrane for separating phenylethanol glycosides of the present invention comprises the following steps:

[0022] Step 1. After soaking the PVDF membrane in methanol solution for 24 hours and activating it, soak it in 0.05mol / L azobisisobutyronitrile / methanol solution for 10 minutes, take out the membrane and put it in an electric blast drying oven at 40°C Take out after drying;

[0023] Step 2: Add 0.2 mmol of verbascoside template molecules and 2 to 8 mmol of functional monomers into the solvent, seal, mix and ultrasonically until the template molecules and functional monomers are completely dissolved, put them into a constant temperature oscillator, and perform pre-polymerization at 30°C and 150rpm 2h, obtain prepolymerization reaction solution;

[0024] Wherein, the functional monomer is one of 4-vinylpyridine, methacrylic acid and acrylamide.

[0025] The solvent is acetonitrile:N,N-dimethylformamide (1:1.5, v / v).

...

Embodiment 1

[0031] Preparation of phenylethanol glycoside molecularly imprinted membrane:

[0032] Step 1. Soak the PVDF membrane in methanol solution for 24 hours, then soak it in 0.05mol / L azobisisobutyronitrile / methanol solution for 10 minutes, take out the membrane and put it in an electric blast drying oven to dry at 40°C remove after drying;

[0033] Step 2. Add 0.2mmol verbascoside as a template molecule and 2mmol 4-vinylpyridine as a functional monomer into the solvent, the solvent is acetonitrile: DMF (1:1.5, v / v), mix and ultrasonically put into constant temperature oscillation Pre-polymerization was carried out at 30°C and 150 rpm for 2 hours to obtain a pre-polymerization reaction solution;

[0034] Step 3, adding 6 mmol of ethylene glycol dimethacrylate as a crosslinking agent and 0.1 mmol of azobisisobutyronitrile as an initiator to the prepolymerization reaction solution obtained in step 2, and mixing uniformly and ultrasonically for 10 minutes to obtain a film casting sol...

Embodiment 2

[0040] The preparation of the phenylethanol glycosides molecularly imprinted membrane was different from Example 1 in that: methacrylic acid was the functional monomer, and the amount of the functional monomer was 2 mmol.

[0041] Selective adsorption experiment of the above-mentioned phenylethanol glycosides molecularly imprinted membrane on Cistanche tubulosa extract: put the molecularly imprinted membrane in a 50mL Erlenmeyer flask, add Cistanche tubulosa extract, seal and place on a shaker at 200rpm, shake at 30°C Adsorption for 24h. The content of purified verbascoside was determined by HPLC. The adsorption capacity of purified verbascoside reached 8.86 mg / g, the adsorption capacity of echinacoside reached 7.83 mg / g, and the selectivity was 1.03.

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Abstract

The invention provides a preparation method of a molecularly imprinted membrane for separation of phenylethanoid glycosides. The method includes the steps of: adding acteoside and a functional monomerinto a solvent, performing sealing, conducting mixing, and carrying out pre-polymerization; and adding ethylene glycol dimethacrylate and azodiisobutyronitrile into the pre-polymerized system to obtain a polymerization system, immersing a PVDF membrane into the polymerization system, carrying out nitrogen bubbling deoxygenation, then carrying out polymerization reaction to obtain an imprinted membrane, and eluting template molecules in the imprinted membrane with an eluent to obtain the molecularly imprinted membrane. According to the invention, by applying the molecularly imprinted membraneto extract active ingredients in cistanche tubulosa, the adsorption capacity of acteoside reaches 62.82mg / g, the adsorption capacity of echinacoside reaches 29.49mg / g, and the selectivity is 2.74. Inpermselectivity experiment, the permeability coefficient of acteoside is 4.02*10<-6>cm<2> / s, the permeability coefficient of echinacoside is 1.07*10<-5>cm<2> / s, and the permeation selectivity factor is 2.65.

Description

technical field [0001] The invention relates to a preparation method of a molecularly imprinted membrane, in particular to a preparation method and application of a molecularly imprinted membrane for separating phenylethanol glycosides. Background technique [0002] Cistanche cistanche belongs to the subclass Synpetalum, order Tubularflowers, and Cistanche cistanche plants of the family Ledanceae. Cistanche deserticola is one of the most valuable tonic Chinese herbal medicines, known as "desert ginseng" and "treasure in medicine". Cistanche tubulosa is mainly produced in southern Xinjiang. It is a desert parasitic plant and is relatively easy to cultivate artificially. Studies have shown that the active ingredients in cultivated and wild Cistanche tubulosa are basically the same, mainly phenylethanol glycosides, polysaccharides, oligosaccharide flavonoids, polyphenols, and proteins. Pharmacological studies have shown that phenylethanol glycosides have the functions of prot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J7/16C08F259/08C08F226/06C08F220/06C08F220/56C08F222/14B01D71/34B01D67/00C08L27/16
CPCB01D67/0006B01D71/34C08F259/08C08J7/16C08J2327/16C08F226/06C08F220/06C08F220/56
Inventor 李雪琴赵小宾郭瑞丽魏忠
Owner SHIHEZI UNIVERSITY
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