Method for separating effective constituent butenolide II from astraolylis lancea formalyrata volatile oil

A technique for volatile oil of Atractylodes Rhizoma and Atractylodes Rhizoma Lactone is applied in the field of traditional Chinese medicine, and can solve the problems of material yield, low purity, difficult separation, loss of material and the like, and achieve the effects of improving yield and purity, simple operation and low cost.

Inactive Publication Date: 2008-09-17
ZHEJIANG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0007]The content of Atractylodes macrolide II in Atractylodes macrocephala is only 0.07% (Li Wei. Effective substances and quality research of Atractylodes macrocephala. Nanjing: Nanjing University of Traditional Chinese Medicine, 2001, 38.) , and it is difficult to separate
The separation method commonly used in the prior art is high-speed counter-current chromatographic separation (Chunxia Zhao, Chaohong He.Preparative isolation and purification of atractyl on and atractylenolide III from the Chinese medicinal plant Atractylodesmacrocephala by high-speed counter-current chromatography.J.Sep.Sci...

Method used

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  • Method for separating effective constituent butenolide II from astraolylis lancea formalyrata volatile oil
  • Method for separating effective constituent butenolide II from astraolylis lancea formalyrata volatile oil
  • Method for separating effective constituent butenolide II from astraolylis lancea formalyrata volatile oil

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Dry the rhizome of Atractylodes macrocephala naturally, crush it into coarse powder of Atractylodes macrocephala, soak it twice with 5 times the volume of ethyl acetate (in a constant temperature water bath at 60°C, stirring at a speed of 500r / min, for 1 hour each time), and concentrate to obtain a yellow-brown volatile oil. After standing for a period of time to make it fully oxidized, extract with a mixed solution of n-hexane-ethyl acetate-ethanol-water in the ratio of 4:1:4:1, take the upper phase and concentrate to obtain a refined volatile oil. The refined volatile oil is separated with 60-100 mesh silica gel in a Φ1.0×40cm chromatographic column, and firstly removed with petroleum ether-ethyl acetate mixed solvent at an elution gradient of 300:1 and a flow rate of 5ml / min Impurity peaks, and then elute with a mixed solvent of petroleum ether-ethyl acetate at an elution gradient of 50:1 and a flow rate of 1ml / min, collect the corresponding fractions, concentrate, an...

Embodiment 2

[0028] Naturally dry the Rhizome of Atractylodes Rhizome, crush it into coarse powder of Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizome, and leaching twice with a mixed solvent made of 5 times the volume of petroleum ether-ethyl acetate in a ratio of 1:1 (60°C constant temperature water bath, stirring speed 500r / min, 1h each time), after standing for a period of time to make it completely oxidized, extract with a mixed solution prepared in the ratio of n-hexane-ethyl acetate-ethanol-water in the ratio of 4:1:4:1, take the upper phase and concentrate to obtain Refined volatile oil. The refined volatile oil is separated with 60-100 mesh silica gel in a Φ1.0×40cm chromatographic column, and firstly removed with petroleum ether-ethyl acetate mixed solvent at an elution gradient of 300:1 and a flow rate of 5ml / min Impurity peaks, and then elute with a mixed solvent of petroleum ether-ethyl acetate at an elution gradient of 50:1 and a flow rate ...

Embodiment 3

[0030] Dry the rhizome of Atractylodes Rhizome naturally, crush it into coarse powder of Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizome, soak twice with a mixed solvent made of 5 times the volume of petroleum ether-ethyl acetate at a ratio of 40:1 (60°C constant temperature water bath, stirring speed 500r / min, 1h each time), after standing for a period of time to make it completely oxidized, extract with a mixed solution prepared in the ratio of n-hexane-ethyl acetate-ethanol-water in the ratio of 4:1:4:1, take the upper phase and concentrate to obtain Refined volatile oil. The refined volatile oil is separated with 60-100 mesh silica gel in a Φ1.0×40cm chromatographic column, and firstly removed with petroleum ether-ethyl acetate mixed solvent at an elution gradient of 300:1 and a flow rate of 5ml / min Impurity peaks, and then elute with a mixed solvent of petroleum ether-ethyl acetate at an elution gradient of 50:1 and a flow rate of 1ml / ...

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Abstract

The invention discloses a method for separating effective component, atractylenolide II, from Rhizoma Atractylodis Macrocephalae volatile oil. The method includes pulverizing rhizome of dried Rhizoma Atractylodis Macrocephalae, extracting in medium and low polar solvents, and concentrating to obtain tan volatile oil; standing for a certain time, extracting the volatile oil with mixed solution prepared from n-hexane, ethyl acetate, ethanol and water at a certain ratio, collecting upper layer phase, and concentrating to obtain the refined volatile oil; and gradient eluting with mixed solvent of petroleum ether and ethyl acetate at a certain ratio with column chromatography, collecting correspondent fraction, concentrating, and recycling solvent to obtain atractylenolide II. The method performs pretreatment on Rhizoma Atractylodis Macrocephalae volatile oil coarse product by extracting and oxidizing before separating through column chromatography to have simple process and low cost, increased yield and purity of atractylenolide II, and avoids the disadvantages in the conventional post-treatment steps such as crystal loss caused by recrystallization, etc.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicines, and in particular relates to a method for separating the active ingredient atractylodes lactone II from the volatile oil of atractylodes rhizome. Background technique [0002] Atractylodes macrocephala koidz (Atractylodes macrocephala koidz), also known as Yushu, Dongzhu, Zheshu, etc., is a perennial herb and a medicinal plant of the Atractylodes genus in the family Asteraceae. Its rhizomes can be used as medicine. Atractylodes macrocephala is warm in nature, sweet and bitter in taste, and belongs to the spleen and stomach meridians, and has the functions of invigorating the spleen and replenishing qi, drying dampness and promoting diuresis, antiperspirant, and preventing miscarriage. It is mainly produced in Zhejiang, Anhui and other places, with the largest output in Yinxian and Xinchang of Zhejiang. It is mainly used for spleen deficiency, indigestion, abdominal distension and dia...

Claims

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Application Information

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IPC IPC(8): C07D307/92A61K36/284
Inventor 王霏娜何潮洪赵春霞雷照沈剑
Owner ZHEJIANG UNIV
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