Method of separating preparation of volatile components from acorus tatarinowii

A technology for volatile components and calamus, applied in the field of medicine, can solve the problems of cumbersome steps, high cost, complicated operation, etc., and achieve the effects of reducing the loss of volatile components, avoiding long-term heating, and simple recovery process

Inactive Publication Date: 2015-12-09
GUANGZHOU XIANGXUE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in view of the difficulty in preparing volatile monomeric compounds, so far, the China Institute for the Control of Pharmaceutical and Biological Products has not yet provided β-asarone and γ-asarone reference substances, and there are β-asarone reference substances sold by individual companies on the market The price of the product is high, the purity is low, and γ-asarone has not been sold. This situation directly affects the research on the medicinal materials of Shichangpu
[0005] In the prior art, there is a method of gradient elution on a silica gel column to prepare β-asarone, but the steps are cumbersome, the yield is low, and the cost is high; the prior art also discloses a "method for refining β-asarone", which requires The β-asarone with a purity of 97.89% to 99.45% can be obtained by repeated crystallization three times at different temperatures, but this method takes a long time, the operation is complicated, and the β-asarone used for refining the volatile oil of Acorus calamus is required to be relatively high. The content is not less than 60%; and the preparation method of γ-asarone has not yet been seen

Method used

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  • Method of separating preparation of volatile components from acorus tatarinowii
  • Method of separating preparation of volatile components from acorus tatarinowii
  • Method of separating preparation of volatile components from acorus tatarinowii

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Take the coarse powder of Acorus calamus, prepare the volatile oil of Acorus calamus by steam distillation, dissolve it in n-hexane to obtain the sample solution to be separated, and inject it into the preparative SFC separation system by an autosampler. The separation conditions are as follows:

[0040] The size of the chromatographic column is Φ19×100mm, the silica gel filler, the particle size is 3-50μm; the mobile phase is CO 2 and modifying agent isopropanol, wherein, the volume ratio of the modifying agent is 10%; the flow rate is 10mL / min; the temperature is 60° C.; the pressure is 100 bar.

[0041] The ultraviolet photometric detector used for online detection, the detection wavelength is 288nm, and the peak fractions of α-asarone, β-asarone and γ-asarone were collected respectively, and the purity was analyzed by GC: α-asarone>98.3% , β-asarone>98.1%, γ-asarone>99.3%, calculated by the weight of volatile oil, the total yield of the three compounds is 77.1%. Ex...

Embodiment 2

[0042] Take the coarse powder of Acorus calamus, prepare the volatile oil of Acorus calamus by steam distillation, dissolve it with n-hexane to obtain the sample solution to be separated, and inject it into the preparative SFC separation system by an autosampler, the conditions are as follows:

[0043] The size of the chromatographic column is Φ19×150mm, the silica gel filler, the particle size is 3-50μm; the mobile phase is CO 2 and modifying agent isopropanol, wherein, the volume ratio of the modifying agent is 10%; the flow rate is 30mL / min; the temperature is 50°C; the pressure is 150bar.

[0044] The ultraviolet photometric detector used for online detection, the detection wavelength is 288nm, and the peak fractions of α-asarone, β-asarone and γ-asarone were collected respectively, and the purity was analyzed by GC: α-asarone>98.5% , β-asarone>98.3%, γ-asarone>99.5%, calculated by the weight of volatile oil, the total yield of the three compounds is 74.6%. Example 3

Embodiment 3

[0045] Take the coarse powder of Acorus calamus, prepare the volatile oil of Acorus calamus by steam distillation, dissolve it with n-hexane to obtain the sample solution to be separated, and inject it into the preparative SFC separation system by an autosampler, the conditions are as follows:

[0046] The size of the chromatographic column is Φ19×250mm, the silica gel filler, the particle size is 3-50μm, and the mobile phase is CO 2and modifying agent isopropanol, wherein, the volume ratio of the modifying agent is 15%; the flow rate is 20mL / min; the temperature is 40°C; the pressure is 200bar.

[0047] The ultraviolet photometric detector used for online detection, the detection wavelength is 288nm, and the peak fractions of α-asarone, β-asarone and γ-asarone were collected respectively, and the purity was analyzed by GC: α-asarone>98.70% , β-asarone>98.56%, γ-asarone>99.98%, calculated by the weight of volatile oil, the total yield of the three compounds is 79.0%. Example ...

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Abstract

The invention relates to a method of separating preparation of volatile components from acorus tatarinowii, wherein the volatile components can include monomer compounds or a composition thereof. The method comprises following steps: (A) with the volatile components as a raw material, extracting a crude volatile extract from the acorus tatarinowii; (B) dissolving the crude volatile extract in an organic solvent to prepare a sample solution for separating preparation; and (C) performing separating preparation to the solution through super-critical fluid chromatography technology to obtain the acorus tatarinowii volatile components. In the method, the acorus tatarinowii volatile components are separated and prepared through the super-critical fluid chromatography technology, and at the same time, a new approach of preparing [alpha]-asarone, [beta]-asarone and [gamma]-asarone is developed. Through the super-critical fluid chromatography technology, the [alpha]-asarone, the [beta]-asarone and the [gamma]-asarone are prepared synchronously just through simple sample injection and separation at a high purity. The method is high in yield of products, is short in separation time and is high in efficiency.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for separating and preparing volatile components of calamus calamus. Background technique [0002] Shichangpu is the dried rhizome of Acorusstatarinowii Schott, a perennial herb of the Araceae family. It was first recorded in "Shen Nong's Herbal Classic" and listed as a top grade. It is used for epilepsy, convulsions, febrile coma, forgetfulness, senile dementia and other diseases. It is one of the few good medicines for cardiovascular and cerebrovascular diseases. [0003] Modern pharmacological research has found that the volatile oil of Shichangpu has various pharmacological effects such as calming the nerves, anti-convulsions, improving intelligence and anti-aging, and is one of the main effective parts of Shichangpu. At present, there are few studies on the separation and preparation of volatile components of Shichangpu, especially its monomer compounds are diffic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/34C07C41/36C07C41/38C07C43/215A61K36/888
CPCA61K36/888C07C41/34C07C41/36C07C41/38C07C43/215Y02P20/54
Inventor 伍军孟鹤范真谢小燕申小花连林生张健
Owner GUANGZHOU XIANGXUE PHARMA CO LTD
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