Preparation method and application of iridoid multi-component imprinted composite material

A technology for iridoids and composite materials, applied in separation methods, chemical instruments and methods, alkali metal compounds, etc., can solve the problems of less imprinted polymers, achieve high separation capacity, reduce production costs, and product recovery rates high effect

Inactive Publication Date: 2020-02-18
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the use of metal-organic framework materials for chromatographic immobilization is a current research hotspot, but

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Preparation and sulfonylation of MIL-101: In 50mL of deionized water, add 1.0mmol of chromium nitrate nonahydrate and 1.5mmol of terephthalic acid, then add 0.3mL of hydrofluoric acid. The solution was poured into a 100mL hydrothermal reaction kettle, sealed and reacted at 493K for 10.5 hours. After cooling, it was filtered with suction, and the solid was washed with deionized water and N,N-dimethylformamide (DMF) successively, and the solid was transferred to Add 50mL ethanol to the reaction kettle, react at 373K for 17 hours, filter and wash repeatedly with ethanol, vacuum dry, grind and sieve to obtain green solid powder MIL-101 (A); put 4.0 g MIL-101 into a 250mL flask , add 100mL CH 3 NO 2 , after stirring evenly, add 5.0 mmol of concentrated sulfuric acid and 6.0 mmol of trifluoromethanesulfonate, react at 308K for 7 hours, filter, wash the solid repeatedly with 50 mL of absolute ethanol and deionized water for 3 times, and dry in vacuo to obtain a solid b. ...

Embodiment 2

[0022] (1) Preparation and sulfonylation modification of MIL-101: In 50mL deionized water, add 1.0mmol chromium nitrate nonahydrate and 2.3mmol terephthalic acid, then add 0.4mL hydrofluoric acid, and mix with ultrasonic stirring The solution was poured into a 100mL hydrothermal reaction kettle, sealed and reacted at 493K for 11.5 hours. After cooling, it was filtered with suction, and the solid was washed with deionized water and N,N-dimethylformamide (DMF) successively, and the solid was transferred to Add 50mL ethanol to the reaction kettle, react at 373K for 19 hours, filter and wash repeatedly with ethanol, vacuum dry, grind and sieve to obtain green solid powder MIL-101 (A); put 4.0 g MIL-101 into a 250mL flask , add 100mL CH 3 NO 2 , after stirring evenly, add 5.0 mmol concentrated sulfuric acid and 9.0 mmol trifluoromethanesulfonate, react at 308K for 8.5 hours, filter, wash the solid repeatedly with 50 mL of absolute ethanol and deionized water for 3 times, and dry i...

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Abstract

The invention discloses a preparation method of iridoid multi-component simultaneous imprinted composite material microspheres and application of the iridoid multi-component simultaneous imprinted composite material microspheres in solid-phase extraction of antihypertensive active compounds in eucommia ulmoides crude extracts. The preparation method comprises the following steps: preparing a metalorganic framework material MIL-101, performing sulfonylation modification and preparing the imprinted composite material. According to the invention, a sulfonic group modified metal organic frameworkis used as a carrier; and multi-component iridoid compounds, namely pinoresinol diglucoside, aucubin and geniposide, as common templates are taken to prepare the imprinted composite microspheres withthe particle size of 20-50 mu m. The material has efficient separation capacity for the antihypertensive compounds in the eucommia ulmoides crude extracts, the imprinted composite microspheres can beused for classifying and purifying the compounds in plants, the imprinted microspheres can be repeatedly used after being recycled, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of new materials, and in particular relates to a preparation method of novel imprinted microspheres with high selective adsorption capacity for multi-component compounds of eucommia iridoids and solid phase extraction separation and purification. Background technique [0002] Eucommia ulmoides is a precious Chinese medicinal material in my country, which has biological activities such as lowering blood pressure. Among them, iridoid compounds, such as pinoresinol diglucoside, are typical blood pressure-lowering biomass. Improving immunity, improving learning and memory, anti-tumor, lowering blood sugar, relieving alcohol, etc., are widely used in clinical applications. Extraction and separation from Eucommia ulmoides is the main way to obtain iridoids. However, some existing extraction techniques often make the extraction process very complicated and the extraction cost remains high due to the insufficient selectivity ...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/10
CPCB01D15/10B01J20/268B01J20/28016
Inventor 李辉田海希毛琳周丽慧欧美婧曲妍
Owner JISHOU UNIVERSITY
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