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Method for preparing eriocalyxin B

A kind of technology of eriophyllin and echinococcinus, which is applied in the field of pharmacy

Active Publication Date: 2010-08-18
KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, in the prior art, there is no report on the method of preparing high-purity pharmaceutical compound echinacea by high-speed countercurrent chromatography (HSCCC)

Method used

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  • Method for preparing eriocalyxin B
  • Method for preparing eriocalyxin B
  • Method for preparing eriocalyxin B

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 1. The preparation of the crude product of Eriophyllin:

[0019] Take 1 kg of the above-ground part of Calyx spp., put it in a 10-liter percolation tank after crushing, extract 3 times by diafiltration at room temperature with 10 liters of 95% ethanol (3 times share 20 liters), and combine the percolation extracts (about 15 liters). liter), concentrated in a spherical concentrator to obtain 67.8 grams of extract, added 120mL of water and stirred evenly, and the aqueous phase was extracted with the same volume of ethyl acetate (V:V=1:1, extracted three times) to obtain ethyl acetate Part 62.7 grams; this extract is dissolved in 95% ethanol, after filtering, put on the MCI column to remove the pigment, flush the column with 90% ethanol, and wash the column with acetone after the fraction containing echinoceline is washed. After concentration of the fraction containing calyxin, 58.8 grams of the crude extract of calyx sp.

[0020] 2, the preparation of calyxin B:

[0021...

Embodiment 2

[0025] A semi-preparative TBE-300B high-speed countercurrent chromatograph is used, equipped with a plunger pump, injection valve, ultraviolet detector and recorder, and the column capacity of multi-layer wound polytetrafluoroethylene is about 260mL. The solvent system was n-hexane / ethyl acetate / methanol / water 5:5:5:5 for the separation and preparation of echinacetin monomer. Firstly, the above-mentioned solvent system was arranged in a separatory funnel, shaken evenly and allowed to stand to separate into layers. After equilibrating for a period of time, separate the upper phase and the lower phase, and take the upper phase as the stationary phase and the lower phase as the mobile phase. Take 500 mg of the crude extract of Calyx sphaericus and dissolve it in the mixture of 5 mL of the upper phase and 5 mL of the lower phase for use. First fill the entire column with the stationary phase; adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column...

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Abstract

The invention relates to a method for preparing eriocalyxin B with high purity from crude extract of lamiaceae plectranthus genus plant flower thinning isodon eriocalyx by applying high speed counter-current chromatography, which is characterized in that two solvent systems which are not mixed and dissolved with each other are applied for separating and purifying natural products in a support tube in a way of high-speed planetary motion, so that irreversible adsorption is not available, the method has the advantages of no loss of sample, no pollution, high efficiency, high speed and large amount of separation, the obtained eriocalyxin B has the purity of more than 98%, and method is applicable to separating and preparing eriocalyxin B monomer from flower thinning isodon eriocalyx crude product prepared under various technical conditions and is suitable for separating and preparing the eriocalyxin B monomer by using counter current chromatographs with various models. The preparation method has simple operation, less separating steps, high efficiency, low loss of solvent and high product purity, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to a method for preparing a high-purity medicinal compound echinophyllin from the crude extract of Calyx spp. Background technique [0002] Laxiflora is a kind of Lamicalyx (Isodon eriocalyx (Dunn) Hara) and Laxiflora (Isodon eriocalyx var. laxiflora C.Y.Wu et H.W. En-kauranes purified from Li). Folkly used for anti-inflammatory and antibacterial. In the Chinese patent application number CN02134163.X, the compound echinophyllin was isolated from Chacalyx maculatum for the preparation of medicaments for preventing or treating cancer. According to the Chinese application number CN200510110089.8, the calyx calyx can also be used to treat diseases such as acute leukemia and Burkitt's lymphoma. Previously reported extraction and separation of eelin mainly adopts column chromatography, including silica gel column and gel column. However, all of these column chromatography require the use of so...

Claims

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Application Information

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IPC IPC(8): C07D493/10B01D15/18B01D15/20
Inventor 孙汉董韩全斌普建新
Owner KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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