Method for preparing harpagoside and sibirioside A by using high-speed counter-current chromatography through separation and purification

A technology of high-speed countercurrent chromatography and zalongin, which is applied in the field of separation of natural medicines, can solve the problems of time-consuming, labor-intensive, environmental pollution, irreversible adsorption, etc., and achieve good separation effect, less solvent consumption and easy operation.

Active Publication Date: 2014-06-25
江苏凯元科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The existing technology generally adopts traditional separation methods such as ordinary chromatographic column method and recrystallization to separate effective monomers in plants, which is not only time-consuming and labor-intensive, but also pollutes the environment, and all fixed relative samples have irreversible adsorption

Method used

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  • Method for preparing harpagoside and sibirioside A by using high-speed counter-current chromatography through separation and purification
  • Method for preparing harpagoside and sibirioside A by using high-speed counter-current chromatography through separation and purification
  • Method for preparing harpagoside and sibirioside A by using high-speed counter-current chromatography through separation and purification

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1. Take 50g of Radix Scrophulariae and crush it into coarse powder, add 500mL of ethanol with a volume fraction of 50% and heat and reflux for extraction for 3 times, extracting for 1 hour each time, combine the extracts and filter, cool to room temperature, and depressurize the filtrate in a rotary evaporator to Without alcohol, the ethanol extract is obtained, and its high-performance liquid chromatogram is as follows figure 1 shown.

[0036] 2. After dispersing 4.1g ethanol extract with 30mL water, add it to AB-8 macroporous adsorption resin column chromatography. After the adsorption is completed, use 5 times the column volume of water → 30% ethanol → 50% ethanol → 70% ethanol →Elute with 95% ethanol solution, collect the ethanol eluate containing the target products harpagoside and sapagoside A, concentrate under reduced pressure to no alcohol, and dry to obtain the mixed crude extract of harpagoside and sapagoside A , see HPLC diagram figure 2 . (% means volum...

Embodiment 2

[0044] 1. Take 50g of Radix Scrophulariae and crush it into a coarse powder, add 500mL of ethanol with a volume fraction of 50% and heat to reflux for extraction for 3 times, each extraction for 1h, combine the extracts, filter, and cool to room temperature. The filtrate was reduced to alcohol-free with a rotary evaporator to obtain ethanol extract and ethanol extract.

[0045] 2. After dispersing 10.2g ethanol extract with 40mL water, add it to AB-8 macroporous adsorption resin column chromatography. After the adsorption is completed, use 5 times the column volume of water → 30% ethanol → 40% ethanol → 50% ethanol → 60% ethanol → 70% ethanol → 95% ethanol solution elution, collect the ethanol eluate containing the target products harpagoside and zalongoside A, concentrate under reduced pressure to no alcohol, and dry to obtain harpagoside and zalongoside Mixed crude extracts of glucoside A.

[0046] 3. Apply high-speed countercurrent chromatography to separate and purify the...

Embodiment 3

[0050] 1. Scrophulariaceae medicinal material extraction is the same as embodiment 1.

[0051] 2. After dispersing 10.3g ethanol extract with 40mL water, add it to AB-8 macroporous adsorption resin column chromatography. After the adsorption is completed, use 5 times the column volume of water → 10% ethanol → 30% ethanol → 40% ethanol → 60% ethanol → 95% ethanol solution for elution, collect the ethanol eluate containing the target products harpagoside and zalongoside A, concentrate under reduced pressure to no alcohol, and dry to obtain harpagoside and zalongoside A. Combine the crude extracts.

[0052] 3. Apply high-speed countercurrent chromatography to separate and purify the crude extract. Take n-butanol, ethyl acetate and water, mix them at a volume ratio of 1:9:10, mix well and let stand, separate the upper and lower phases, remove the upper phase as the stationary phase, and the lower phase as the mobile phase, fill the stationary phase with high-speed For the multi-...

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Abstract

The invention discloses a method for preparing harpagoside and sibirioside A by using high-speed counter-current chromatography through separation and purification. The method comprises the steps of crushing a radix scrophulariae medicinal material, extracting by ethanol, and enriching by using macro-porous adsorption resin to obtain a crude extract; performing high-speed counter-current chromatography separation on the crude extract; forming a high-speed counter-current solvent system by using a solvent A, a solvent B and a solvent C of which the volume ratio is (1-5): (5-10): (1-10), wherein the solvent A is methanol, ethanol, n-butyl alcohol or isobutanol; the solvent B is ethyl acetate, propyl acetate or n-butyl acetate; the solvent C is water; an upper phase is a stationary phase, and a lower phase is a mobile phase, so that harpagoside and sibirioside A are prepared respectively. The method disclosed by the invention is used for preparing harpagoside and sibirioside A by using the high-speed counter-current chromatography, does not have irreversible adsorption, avoids the loss of samples, and has the characteristics of good separation effect, small solvent dose, no pollution, high efficiency and high speed.

Description

(1) Technical field [0001] The invention belongs to the field of separation of natural medicines, and relates to a method for separating and purifying harpagoside and harpagoside A, in particular to a method for separating and purifying high-purity harpagoside and rapagoside A by high-speed countercurrent chromatography. (2) Background technology [0002] Scrophulariaceae is the dried root of Scrophularia ningpoensis Hemsl, a plant of the family Scrophulariaceae. Traditional Chinese medicine believes that Scrophulariaceae is sweet, bitter, and salty, and its nature is slightly cold. It has the effects of nourishing yin and cooling blood, purging fire and detoxifying, etc. It is a traditional Chinese medicine commonly used in clinical practice. [0003] Modern medicine shows that Scrophulariaceae contains terpenoids, glycosides, alkaloids and other ingredients, which have anti-inflammatory, anti-tumor, and liver-protecting effects. [0004] Harpagoside is an iridoid substan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H13/04C07H17/04C07H15/203
Inventor 李行诺童胜强颜继忠张文强
Owner 江苏凯元科技有限公司
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