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Method for preparing atractylon

The technology of Atractylodes atractylodes and Atractylodes atractylodes, which is applied in the field of preparation of Atractylodes atractylodes, can solve the problems of cumbersome operation, unfavorable industrial scale-up, unfavorable industrialized operation, etc., and achieve the effects of less pollution, less energy consumption, and favorable large-scale production operations

Inactive Publication Date: 2010-09-01
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there are few reports about the preparation process of atractylone, and it is often not conducive to industrial operation. For example, a preparation method of atractylone is disclosed in Chinese patent document CN100551366C: the medicinal material is separated and purified by silica gel chromatography after extraction, and the operation Complicated, not conducive to industrial scale-up

Method used

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  • Method for preparing atractylon

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Effect test

Embodiment 1

[0015] Get 10Kg of dry rhizome of Atractylodes atractylodes, crush, add to CO 2 In the supercritical extractor, n-hexane is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 1%, the extraction pressure is 30MPa, the temperature is 40°C, and CO 2 The flow rate is 10L / min, the extraction time is 60min, and the extract is injected into a molecular still for two-stage molecular distillation. The evaporation surface temperature of the first stage distillation is 60°C, the pressure is 100Pa, the distillation time is 40min, and the distillate is collected. Carry out the second-stage distillation, the temperature of the evaporation surface is 30°C, the pressure is 60Pa, distill for 40min, collect the distillate, add acetone, refrigerate and crystallize, separate and crystallize, wash and dry to obtain 22.5g of atractylone, which is detected by HPLC. was 98.3%.

Embodiment 2

[0017] Get 10Kg of dry rhizome of Atractylodes atractylodes, crush, add to CO 2 In the supercritical extractor, n-hexane is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 4%, the extraction pressure is 60MPa, the temperature is 60°C, and the CO 2 The flow rate is 30L / min, the extraction time is 120min, and the extract is injected into a molecular still for two-stage molecular distillation. The evaporation surface temperature of the first stage distillation is 90°C, the pressure is 150Pa, the distillation time is 80min, and the distillate is collected. Carry out the second-stage distillation, the temperature of the evaporation surface is 50°C, the pressure is 80Pa, distill for 80min, collect the distillate, add acetone, refrigerate and crystallize, separate and crystallize, wash and dry to obtain 25.5g of atractylone, which is detected by HPLC. was 97.7%.

Embodiment 3

[0019] Get 10Kg of dry rhizome of Atractylodes atractylodes, crush, add to CO 2 In the supercritical extractor, n-hexane is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%, the extraction pressure is 50MPa, the temperature is 50°C, and the CO 2 The flow rate is 20L / min, the extraction time is 80min, and the extract is injected into a molecular still for two-stage molecular distillation. The evaporation surface temperature of the first stage distillation is 80°C, the pressure is 120Pa, the distillation time is 60min, and the distillate is collected. Carry out the second-stage distillation, the temperature of the evaporation surface is 40°C, the pressure is 70Pa, distill for 60min, collect the distillate, add acetone, refrigerate and crystallize, separate and crystallize, wash and dry to obtain 23.8g of atractylone, which is detected by HPLC. was 98.9%.

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Abstract

The invention relates to a method for preparing atractylon, which has the characteristic of simple and convenient operation, light pollution and low energy consumption. The method comprises the following process steps of: selecting a dry rhizome of plants, such as atractylis lancea, atractylodes chinensis and rhizoma atractylodis macrocephalae, crushing the rhizome, and adding the rhizome into a CO2 super critical extractor for extracting to obtain an extract; injecting the extract into a molecular distillation apparatus, and then performing two-grade molecular distillation on the extract in the molecular distillation apparatus, wherein the temperature of an evaporating surface of a first grade distillation is between 60 and 90 DEG C, the pressure is 100 to 150Pa, and the distillation time is 40 to 80 minutes; collecting distillate, and then performing a second grade distillation on the distillate, wherein the temperature of the evaporating surface is between 30 and 50 DEG C, the pressure is 60 to 80Pa, and the distillation time is 40 to 80 minutes; and then collecting the distillate, adding acetone, refrigerating, crystallizing, separating a crystal, washing and drying the crystal to obtain the product. The atractylon prepared by the method has high purity, and the industrial amplification is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of atractylone, in particular to a preparation method for extracting atractylone from plants. Background technique [0002] Atractylon, also known as: Atractylodes ether, molecular formula: C 15 h 20 O, molecular weight: 216.322, CAS accession number: 6989-21-5, mainly found in Compositae plants Atractylodes lancea (Thunb.) DC., Atractylodes chinensis (DC.) Koidz, Atractylodes macrocephala Koidz., etc. in the rhizomes of various plants. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that atractylodes has various pharmacological activities such as liver protection, anti-oxidation, anti-inflammation, anti-tumor, and anti-influenza virus. [0005] In the prior art, there are few reports about the preparation process of atractylone, and it is often not conducive to industrial operation. For example, a preparation method of atractylone is disclosed in Chinese patent docum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/92
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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