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Method for preparing large-head atractylodes rhizome and sesquiterpene compound

A technology of sesquiterpene and compound, which is applied in the field of preparation of Atractylodes sesquiterpene compound by supercritical extraction coupling fractionation technology, which can solve problems such as complex process and removal of monoterpene compounds, achieve low temperature, maintain biological activity, and not easily Effects of Oxidation and Degradation Reactions

Inactive Publication Date: 2011-02-23
SHENZHEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent "Atractylodes ketone, plants containing atractylodes ketone and the use of atractylodes ketone extract in the preparation of anti-influenza virus drugs" (CN1857358A) discloses a method using supercritical CO 2 Method for extracting atractylodes ketone from atractylodes herb without removing monoterpene compounds therein
Although these patents use the supercritical extraction method, due to the supercritical CO 2 While extracting sesquiterpene components such as atractylone, some volatile small molecule monoterpene components are also extracted. If further purification is required, multiple column chromatography is involved, and the process is complicated

Method used

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  • Method for preparing large-head atractylodes rhizome and sesquiterpene compound

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 Preparation of Deterpenes and Sesquiterpene Compounds of Atractylodes Rhizome Volatile Oil

[0030] 1. Extraction and fractionation process of Atractylodes macrocephala volatile oil

[0031] Atractylone reference substance, provided by Shenzhen Neptunus Biological Co., Ltd.

[0032] Experimental device: supercritical CO 2 The extraction and fractionation equipment is manufactured by Jiangsu Huaan Supercritical Company, and the device is made of CO 2 It is composed of supply system, extractor, fractionation column and separator. The volume of the extractor is 1L, the height of the fractionation column is 2m, and the inner diameter is 20mm. The column is filled with stainless steel foil and divided into four sections for temperature control. Valves V1 and V2 control the pipes connecting the extractor, fractionation column and separator, and valve V3 controls the pressure of the fractionation column. The entire system can withstand a maximum pressure of 35M...

Embodiment 2

[0042] The extraction of embodiment 2 Atractylodes macrocephala volatile oil

[0043] This example examines the extraction process of Atractylodes macrocephala volatile oil. Put 200g of Atractylodes macrocephala medicinal material into the liner of the extractor, and seal it. Open CO 2 Cylinder, CO 2 After the gas is cooled into a liquid by the cooler 3, it is pressurized by the high-pressure metering pump 4 and enters the extractor 6. After extracting the volatile oil under the extraction conditions of 25MPa and 308K, open the valve V1, close the valve V2, supercritical CO 2 The volatile oil is carried into the separator 10 for analysis at 5MPa and 323K. CO 2 The flow rate is controlled at 5L / min, and is emptied through the rotameter 12. The extracted volatile oil was collected, and the contents of monoterpene and atractylone in the components were determined by gas chromatography, and the results are shown in Table 2.

[0044] Table 2 Supercritical Extraction of Atr...

Embodiment 3

[0047] Example 3 The influence of extraction pressure on the extraction of Atractylodes macrocephala volatile oil

[0048] This example examines the effect of extraction pressure on the volatile oil of Atractylodes macrocephala. Put 200g of Atractylodes macrocephala medicinal material into the liner of the extractor, and seal it. By the method and parameter of embodiment 2, under the temperature of 308K, control supercritical CO 2 The pressure was 15-30MPa. After the volatile oil was extracted, the content of monoterpene and atractylone in the fraction was determined by gas chromatography. The results are shown in Table 3.

[0049] Table 3 Effect of extraction pressure on extraction of Atractylodes macrocephala volatile oil

[0050]

[0051] The results of this example show that under lower pressure, the extraction rate of volatile oil is lower, the main components are monoterpene components with lower molecular weight, and the content of atractylone is very low. As th...

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Abstract

The invention discloses a method for preparing a large-head atractylodes rhizome and sesquiterpene compound. The method comprises the following steps of: 1) extracting a large-head atractylodes rhizome medicinal material at a set temperature and under a set pressure in a supercritical extractor, and feeding the extract into a fractionating column along with supercritical CO2 fluid; 2) applying a temperature gradient from low to high to the fractionating column under a certain fractionation pressure to ensure that the supercritical CO2 fluid sectionally fractionates volatile oil at a fixed flow rate; and 3) separating the volatile oil subjected to fractionation into two fractionation sections including a monoterpene component and a sesquiterpene compound, performing pressure reduction and feeding into a separator sequentially, collecting the fractionation section of the sesquiterpene compound, metering the CO2 by a rotor meter and emptying. By the method, the supercritical extraction is coupled to fractionation technology, so that the removal of the terpene from the volatile oil of the large-head atractylodes rhizome in the supercritical CO2 medium and the enrichment of the sesquiterpene are continuously finished, and a new way is provided for preparing the monoterpene-free large-head atractylodes rhizome and sesquiterpene compound.

Description

technical field [0001] The invention belongs to the field of separation and purification of pharmaceutical components, and in particular relates to a method for preparing Atractylodes macrocephala sesquiterpene complex by supercritical extraction coupling fractionation technology. Background technique [0002] Sesquiterpenes are natural terpenoids with 15 carbon atoms in the molecule. The general formula is C 15 h 24 , with a molecular weight of 204. Sesquiterpenes often exist in volatile oils in the form of derivatives such as alcohols, ketones, and lactones in plants. They are the main components of high boiling point parts in volatile oils. Most of them have strong aroma and biological activity. important raw materials. [0003] Atractylodes macrocephala is the dried rhizome of Atractylodes macrocephala koidz, which is one of the most widely used medicinal materials in clinical practice. Traditional Chinese medicine believes that it is warm in nature, pungent and bitt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/284A61K125/00A61P1/16C07D307/92
CPCY02P20/54
Inventor 文震刘波郑宗坤游新奎蒲一涛刘剑洪
Owner SHENZHEN UNIV
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