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Preparation method of atractylenolide II

A technique of atractylodes lactone and high-speed countercurrent chromatography is applied in the field of preparation of atractylodes lactone II, which can solve the problems of high preparation cost, low efficiency, low content of atractylodes lactone II, etc., and achieves a simple enrichment and purification process and improves the utilization rate. Effect

Active Publication Date: 2018-01-09
广东正汇源实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] First, the demand for Atractylodes macrocephala raw materials is large, and the preparation cost is high;
[0007] Second, the content of Atractylodes lactone II is low, and it needs to be separated by column chromatography repeatedly, which is inefficient and not suitable for large-scale production

Method used

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  • Preparation method of atractylenolide II

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Experimental program
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Effect test

Embodiment 1

[0026] 1. Experimental equipment

[0027] TBE-300A high-speed countercurrent chromatograph, China Shanghai Tongtian Biochemical Technology Co., Ltd.: equipped with TBE-2000 ultraviolet detector (polytetrafluoroethylene column, inner diameter 1.6mm, column volume 280mL), TBP-50 pump.

[0028] 2. Experimental methods and results

[0029] A preparation method of atractyloid II, comprising the steps of:

[0030] Step S1, adding acid to rot: Atractylodes macrocephala is crushed through a 40-mesh sieve, and dilute hydrochloric acid is sprayed while stirring. The concentration of dilute hydrochloric acid is 0.3mol / L. After the medicinal powder is wet, it is stacked overnight at 55°C;

[0031] Step S2, ethanol extraction: extract the above-mentioned decomposed medicinal powder with an ethanol solution with a concentration of 75% by volume, the solid-to-liquid ratio is 1:40, the extraction method is cold soaking for 48 hours, the extract is collected, and the ethanol in the extract is...

Embodiment 2

[0044] A preparation method of atractyloid II, comprising the steps of:

[0045] Step S1, adding acid to rot: Atractylodes macrocephala is crushed through a 40-mesh sieve, and dilute hydrochloric acid is sprayed while stirring. The concentration of dilute hydrochloric acid is 0.2mol / L. After the powder is wet, it is stacked overnight at 60°C;

[0046] Step S2, ethanol extraction: extract the above-mentioned decomposed medicinal powder with an ethanol solution with a concentration of 60% by volume, the solid-to-liquid ratio is 1:40, the extraction method is cold soaking for 48 hours, the extract is collected, and the ethanol in the extract is recovered to obtain Concentrate;

[0047] Step S3, macroporous resin enrichment: dilute the concentrated solution with water to a density of 2.5 g / mL, adjust the pH value to 5.2, load the sample on XDA-6 macroporous adsorption resin, and use volume percent concentrations of 25%, 45%, 65%, and 85% ethanol solutions were eluted for 6 column...

Embodiment 3

[0050] A preparation method of atractyloid II, comprising the steps of:

[0051]Step S1, adding acid to rot: Atractylodes macrocephala is crushed through a 40-mesh sieve, and dilute hydrochloric acid is sprayed while stirring. The concentration of dilute hydrochloric acid is 0.4mol / L. After the powder is wet, it is stacked at 50°C overnight;

[0052] Step S2, ethanol extraction: extract the above-mentioned decomposed medicinal powder with an ethanol solution with a concentration of 90% by volume, the solid-to-liquid ratio is 1:40, the extraction method is cold soaking for 48 hours, the extract is collected, and the ethanol in the extract is recovered to obtain Concentrate;

[0053] Step S3, macroporous resin enrichment: dilute the concentrated solution with water to a density of 2.5 g / mL, adjust the pH value to 6.4, load the sample on XDA-6 macroporous adsorption resin, and use volume percentage concentration of 25%, 45%, 65%, and 85% ethanol solutions were eluted for 10 colu...

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Abstract

The invention discloses a preparation method of atractylenolide II. The preparation method comprises the following steps of S1, acid adding and corroding; S2, extracting by ethyl alcohol; S3, enriching by macroporous resin; S4, high-speed reverse chromatography purifying. The preparation method is characterized in that the acid adding and corroding are firstly performed under the acid condition, so that the content of atractylenolide II in the bighead atractylodes rhizome is obviously increased and is increased by 80 times or more; then, the atractylenolide II is selectively enriched by the macroporous adsorption resin, so as to obtain crude extract of the atractylenolide II; finally, the atractylenolide II with purity higher than 98% is obtained by the high-speed reverse chromatography purifying. The preparation method has the advantages that the utilization rate of the bighead atractylodes rhizome is improved, the enriching and purifying technology is simple, the repeated use of silicagel columns is not needed, and the preparation method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of chemistry and relates to the preparation of natural compounds, in particular to a preparation method of atractylodes lactone II. Background technique [0002] Atractylodes lactone Ⅱ is a compound in Atractylodes macrocephala, and Atractylodes lactone Ⅰ and Atractylodes lactone Ⅲ are the main lactone components in Atractylodes rhizome. Its chemical structural formula is as follows, Shengyuanshang Atractylodes lactone III is the oxidation product of Atractylodes lactone I, and Atractylodes lactone II is the dehydration product of Atractylodes lactone III. It is generally believed that Atractylodes lactone Ⅰ and Atractylodes lactone Ⅲ are the main active ingredients of Atractylodes Rhizoma Atractylodes Rhizome, which are anti-inflammatory and anti-cancer active ingredients (Reference: Research Progress of Atractylodes Atractylodes Components and Their Pharmacological Actions, Chinese Pharmacy 2012, No. 23 Volume 39)....

Claims

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Application Information

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IPC IPC(8): C07D307/92
Inventor 王莉张艳峰孙天娇
Owner 广东正汇源实业有限公司
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