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Method for using normal propyl alcohol-seignette salt double-aqueous-phase system to extract, separate and purify phlorizin

A technology of potassium sodium tartrate and two-phase system, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., to achieve the effects of easy integration technology, easy amplification, and low energy consumption

Active Publication Date: 2018-02-23
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the preparation of high-purity phlorizin by using a two-phase aqueous system as an extraction solvent combined with recrystallization technology for high-yield extraction, separation and purification

Method used

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  • Method for using normal propyl alcohol-seignette salt double-aqueous-phase system to extract, separate and purify phlorizin
  • Method for using normal propyl alcohol-seignette salt double-aqueous-phase system to extract, separate and purify phlorizin
  • Method for using normal propyl alcohol-seignette salt double-aqueous-phase system to extract, separate and purify phlorizin

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Get 1000g of Coryne fruticosa leaves (5.62% phlorizin content), pulverize through a 50 mesh sieve, add 10Kg of the two-phase system extraction solvent composed of n-propanol-potassium sodium tartrate-water, and add n-propanol in the two-phase system extraction solvent. The mass fraction of alcohol is 25.75%, the mass fraction of potassium sodium tartrate is 11.00%, the mass fraction of water is 63.25%, microwave-assisted extraction is 30 minutes, extraction temperature is 80 ℃, microwave power is 400W, static phase separation, phase separation The temperature is 30°C, the phase separation time is 4 hours, separate the upper phase, add n-propanol of equal weight, let it stand at 4°C for 48 hours, filter, concentrate the filtrate under reduced pressure, dry the crude phlorizin, and use a recrystallization solvent For recrystallization, the recrystallization solvent was 65% by volume of isopropanol and 35% by volume of water to obtain 44.45 g of phlorizin crystals (transfer...

Embodiment 2

[0061] Get 1000g of Coryne fruticosa leaves (5.62% phlorizin content), pulverize through a 50 mesh sieve, add 10Kg of the two-phase system extraction solvent composed of n-propanol-potassium sodium tartrate-water, and add n-propanol in the two-phase system extraction solvent. The mass fraction of alcohol is 35.26%, the mass fraction of potassium sodium tartrate is 7.97%, the mass fraction of water is 56.77%, microwave-assisted extraction is 30 minutes, extraction temperature is 80 ℃, microwave power is 600W, static phase separation, phase separation The temperature is 30°C, the phase separation time is 2 hours, separate the upper phase, add n-propanol of equal weight, stand at 4°C for 48 hours, filter, concentrate the filtrate under reduced pressure, dry the crude phlorizin, and use a recrystallization solvent Recrystallization, the recrystallization solvent is 65% volume of isopropanol and 35% volume of water, to obtain 46.31 g of phlorizin crystals (82.4% transfer rate).

[...

Embodiment 3

[0065] Get 1000g of Coryne fruticosa leaves (5.62% phlorizin content), pulverize through a 50 mesh sieve, add 10Kg of the two-phase system extraction solvent composed of n-propanol-potassium sodium tartrate-water, and add n-propanol in the two-phase system extraction solvent. The mass fraction of alcohol is 44.88%, the mass fraction of potassium sodium tartrate is 4.88%, the mass fraction of water is 50.24%, microwave-assisted extraction is 30 minutes, extraction temperature is 80 ℃, microwave power is 800W, static phase separation, phase separation The temperature is 30°C, the phase separation time is 4 hours, separate the upper phase, add n-propanol of equal weight, let it stand at 4°C for 48 hours, filter, concentrate the filtrate under reduced pressure, dry the crude phlorizin, and use a recrystallization solvent For recrystallization, the recrystallization solvent was 65% by volume of isopropanol and 35% by volume of water to obtain 47.54 g of phlorizin crystals (transfer ...

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Abstract

The invention provides a preparing method for using microwaves to assist a normal propyl alcohol-seignette salt double-aqueous-phase system in extracting, separating and purifying phlorizin. The preparing method comprises the steps of smashing raw medicinal materials, using a double-aqueous-phase system composed of normal propyl alcohol, seignette salt and water as an extraction solvent to conductmicrowave assisting extraction, conducting phase splitting, removing salt in the upper phase, recycling the solvent to obtain a coarse product of phlorizin, and then conducting recrystallization to obtain a phlorizin crystal, wherein a recrystallization solvent is prepared from, by volume, 65% of isopropanol and 35% of water. The preparing method has the advantages of integrating extraction and leaching, being easy to amplify, capable of being continuously operated, having an integrated technology, and being environmentally friendly, high in phlorizin transfer rate and purity and the like.

Description

technical field [0001] The invention belongs to the technical field of extracting active ingredients of natural products, and relates to a preparation method for extracting, separating and purifying phloridzin by a microwave-assisted n-propanol-potassium sodium tartrate two-phase system. Background technique [0002] The aqueous two-phase system is a two-phase system that is impermeable to each other after two phase-forming substances are fully dissolved in water, under the influence of intermolecular repulsion and steric hindrance, and balanced for a period of time. The current common aqueous two-phase system consists of polymer-polymer-water, polymer-salt-water, ionic liquid-salt-water, small molecule hydrophilic organic solvent-salt-water. Traditional natural product active ingredients are extracted by water or aqueous ethanol, primary metabolites and secondary metabolites coexist, effective and ineffective components coexist, and further refining uses extraction and chro...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08
CPCC07H1/08C07H15/203
Inventor 王威刘小红李国梁孙世伟刘洋韩立春
Owner QINGDAO UNIV
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