Bamboo-leaf-flavonoids molecular imprinted solid-phase extraction column, preparation and application thereof

A solid-phase extraction column and molecularly imprinted technology, which is applied in the field of preparation of bamboo leaf flavonoid molecularly imprinted solid-phase extraction column, can solve problems such as difficulty in meeting the demand for high-content bamboo leaf flavonoid products

Inactive Publication Date: 2012-09-19
INT CENT FOR BAMBOO & RATTAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bamboo leaf flavone products currently on the market are mainly crude products, and the total content of the above four flavonoids is generally within 10%, which is difficult to meet the market demand for high-content bamboo leaf flavonoid products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0025] Example 1. Bamboo leaf flavone molecularly imprinted polymer particle solid-phase extraction column (molar ratio of template molecule to functional monomer is 1:5)

[0026] (1) Prepare a carboxyethyl cellulose solution with a concentration of 3%-3.5%; dissolve 2.5mmol of the functional monomer 4-vinylpyridine (4-vp), 0.5mmol of the template molecule luteolin and 5mmol of zinc acetate in methanol , ultrasonication for 30min; mix 7.5mL of cross-linking agent ethylene glycol dimethacrylate (EGDMA), 0.2g initiator (AIBN) and 7.5mL of xylene; ultrasonication for 20min; mix the above three solutions with ultrasonic Degas for 10 minutes; stir at 650 rpm at 70°C for 10 hours.

[0027] (2) The molecularly imprinted polymer particles prepared above were centrifugally filtered, then washed 5 times with ultrapure water, and washed 5 times with methanol suction filtration, and finally the template molecules were further removed by Soxhlet extraction.

[0028] (3) Vacuum drying (60°...

example 2

[0030] Example 2. Molecularly imprinted polymer particle solid-phase extraction column for bamboo leaf flavonoids (the molar ratio of template molecules to functional monomers is 1:8)

[0031] (1) Prepare a carboxyethyl cellulose solution with a concentration of 3%-3.5%; dissolve 4.0mmol of the functional monomer 4-vinylpyridine (4-vp), 0.5mmol of the template molecule luteolin and 5mmol of zinc acetate in methanol , ultrasonication for 30min; mix 7.5mL of cross-linking agent ethylene glycol dimethacrylate (EGDMA), 0.2g initiator (AIBN) and 7.5mL of xylene; ultrasonication for 20min; mix the above three solutions with ultrasonic Degas for 10 minutes; stir at 650 rpm at 70°C for 10 hours.

[0032] (2) The molecularly imprinted polymer particles prepared above were centrifugally filtered, then washed 5 times with ultrapure water, and washed 5 times with methanol suction filtration, and finally the template molecules were further removed by Soxhlet extraction.

[0033] (3) Vacuu...

example 3

[0035] Example 3. Preparation and performance evaluation of molecularly imprinted solid-phase extraction column for bamboo leaf flavonoids

[0036] ⑴Use a 3mL polypropylene solid-phase extraction column empty tube as the solid-phase extraction column, place a layer of 20 μm polyethylene sieve plate at the bottom of the solid-phase extraction column, and accurately weigh 200 mg of the molecularly imprinted polymer of Example 1 or 2 , dry-packed into a small column, lightly tapped and compacted, and then added a layer of sieve plate to obtain a small column for molecularly imprinted solid-phase extraction of bamboo leaf flavonoids.

[0037] (2) Rinse the column with 2 mL of acetonitrile and keep it for 2 minutes to remove the residual liquid and keep it moist. Do not let the eluent drain before loading the sample;

[0038] (3) Sample loading. Take 10 mL of bamboo leaf extract and add it to a molecularly imprinted solid-phase extraction column. The extract contains luteolin, or...

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Abstract

The invention relates to a bamboo-leaf-flavonoids molecular imprinted solid-phase extraction column, preparation and application thereof, and belongs to the technical field of medicine separation. Template molecule luteolin, functional monomer 4-ethylpyridine and ethylene glycol dimethacrylate which is a cross-linking agent are polymerized into bamboo-leaf-flavonoids molecular imprinted polymer particles in a suspension manner, the molar ratio of template molecules to the functional monomer to the cross-linking agent is 1:(5-8):80. The prepared bamboo-leaf-flavonoids molecular imprinted polymer particles are filled in a polypropylene or glass solid-phase extraction column hollow tube, so that the bamboo-leaf-flavonoids molecular imprinted solid-phase extraction column is prepared. The bamboo-leaf-flavonoids molecular imprinted solid-phase extraction column is used for selectively gathering and purifying bamboo-leaf-flavonoids extracting solution, has the advantages if simplicity, rapidness, high recycling rate and the like, and is wide in application prospect in the field of separation of natural flavonoids compounds.

Description

technical field [0001] The invention belongs to the technical field of medicine separation, and in particular relates to a preparation method of a bamboo leaf flavonoid molecularly imprinted solid-phase extraction column for highly selective separation, purification and enrichment of flavonoids in bamboo leaf extract. Background technique [0002] In the separation of drugs, the pretreatment process of samples is very important. Column chromatography is a commonly used sample pretreatment technique. Solid Phase Extraction (Solid Phase Extraction, SPE) is developed from the combination of liquid-solid extraction and column liquid chromatography. Compared with Liquid-Liquid Extraction (LLE), SPE has high recovery and separation effect. Well, it is widely used in the pretreatment of samples due to its advantages of simple operation, time saving and labor saving. [0003] At present, the types of SPE column packing are normal phase, reversed phase, ion exchange column and adso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01D15/08C07D311/30
Inventor 汤锋岳永德王进姚曦郭雪峰孙嘏王光勇
Owner INT CENT FOR BAMBOO & RATTAN
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