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Industrial production method of high-purity beta-elemi alkene bulk medicament

A technology for elemene and raw materials, which is applied in the field of obtaining high-purity beta-elemene raw materials, can solve the problems of limited raw material sources, complicated production equipment, high cost and the like

Inactive Publication Date: 2009-04-08
沈阳万爱普利德医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a kind of β-elemene containing β-elemene in order to overcome the existing problems in the prior art, such as the limitation of the raw material source of high-content β-elemene, complex and expensive production equipment, and poor extraction stability of instruments and equipment. A new method for the preparation of high-purity β-elemene raw materials from natural plants of ene

Method used

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  • Industrial production method of high-purity beta-elemi alkene bulk medicament
  • Industrial production method of high-purity beta-elemi alkene bulk medicament

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a. Take natural plant medicine turmeric tuber as raw material;

[0027] b. The zedoary turmeric oil is obtained by steam distillation, and the content of β-elemene is 6.0%;

[0028] c. Put the raw material obtained in b into the rectification tower kettle for rectification, control the vacuum degree to 5-6mm Hg, the temperature of the tower kettle is 123℃~124℃, when the reflux ratio is 1:1, the removal temperature is at The impurity fraction below 75°C; the reflux ratio is controlled to be 3:1, and the fraction with a temperature of 77°C to 82°C is collected to obtain β-elemene with a content of 30.0%.

[0029] d. Dilute the 30.0% β-elemene obtained in step c with a double volume of 85% ethanol aqueous solution, and perform column chromatography on the macroporous adsorption resin. First, use a 60% ethanol aqueous solution to continuously flush the column for four If the retention volume is above, flush the column with 70% ethanol water for two retention volumes. The 70% et...

Embodiment 2

[0033] a. Take fresh leaves of natural plant Java citronella as raw materials;

[0034] b. The Java citronella, a medicinal material, is steam distilled to obtain Java volatile oil, in which the content of β-elemene is 5.0%;

[0035] c. Put the raw material obtained in b into the rectification tower kettle for rectification, control the vacuum degree to 2~3mm Hg, the temperature of the tower kettle is 116℃~117℃, when the reflux ratio is 1:1, the removal temperature is at The impurity fraction below 75°C; the reflux ratio is controlled to be 3:1, and the fraction with a temperature of 78°C to 81°C is collected to obtain β-elemene with a content of 16.0%.

[0036] d. Dilute the 16.0% β-elemene obtained in step c with a double volume of 80% ethanol aqueous solution, and perform column chromatography on a 20-fold weight macroporous adsorption resin, first with a 60% ethanol aqueous solution Continuously flush the column with more than four retention volumes, and then flush the column ...

Embodiment 3

[0040] a. Take the fresh leaves of natural plant Solidago canadensis as raw materials;

[0041] b. The volatile oil of Solidago goldenrod leaves is extracted by supercritical extraction, in which the content of β-elemene is 14.3%;

[0042] c. Put the raw material obtained in b into the rectification tower kettle for rectification, control the vacuum to be 6~7mm Hg, the temperature of the tower kettle is 123~124℃, when the reflux ratio is 1:1, the removal temperature is 75 The impurity fraction below ℃; the reflux ratio is controlled to 4:1, and the fraction with a temperature of 79℃~82℃ is collected to obtain β-elemene with a content of 40.6%.

[0043] d. Dilute the 40.6% β-elemene obtained in step c with a 90% ethanol aqueous solution twice the volume, and perform column chromatography on a 20-fold weight macroporous adsorption resin, first using a 60% ethanol aqueous solution Continuously flush the column with more than four retention volumes, and then flush the column with 75% ...

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Abstract

The invention provides a method for preparing high-purity beta elemene from natural plants containing the beta elemene such as curcuma zedoary (earthnuts or tubers of the curcuma zedoary), cedronella (fresh leaves of the cedronella), yellowtop (roots, stems, leaves, flowers and seeds of the yellowtop) and so on, which can improve the production efficiency from starting materials to the high-purity beta elemene and reduce the production cost. Compared with the prior art, the method is mainly different in that the roots, stems, leaves, flowers and seeds of the natural plants are taken as raw materials; oleum volatile of specific parts of the natural plants is obtained by methods for extracting different oleum volatiles, and is rectified by the rectification method to obtain the beta elemene with high content; impurity compositions are removed by the macroporous adsorption resin separation method or macroporous adsorption resin combined with the ethanol extraction method, and the silver nitrate complex extraction method in turn; and finally the beta elemene with the content between 95.0 and 99.9 percent is obtained through reduced pressure distillation or rectification. The bulk pharmaceutical chemicals not only can be prepared into oral dosing preparation such as emulsion oral liquid, self-emulsifying / self-microemulsifying capsules, soft capsules and so on, but also can be prepared into non-alimentary dosing preparation such as emulsion injection, liquid drugs injection, transdermal absorbent, lung sprays, suppository and so on. The method has the advantages of novel design, simple apparatus, concise operating steps, obvious shortened operating time, improvement of the production efficiency and high yield coefficient, and is suitable for industrialized production.

Description

Technical field: [0001] The invention relates to an industrialized production method for obtaining high-purity beta-elemene raw materials. Background technique: [0002] Elemene is isolated from turmeric oil and citronella oil. It has been widely used in the treatment of cancer. The earliest anticancer drug was made into turmeric oil injection from turmeric oil. This injection can only be used locally The way of tumor administration to treat cervical cancer has a long course of treatment and inconvenient administration. However, this injection cannot be used for effective treatment of other cancers. In order to solve the problem of the limitation of the use of turmeric oil injection, people separated elemene with fixed proportions from turmeric oil and citronella oil to make elemene injection. In addition to local tumor administration and regional administration, the emulsion injection can also be injected intravenously. It can treat cervical cancer, brain tumors, malignant tumor...

Claims

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Application Information

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IPC IPC(8): C07C13/19C07C7/00C07C7/04C07C7/12C07C7/10A61K31/01A61P35/00
Inventor 李淑斌孙敏鸽周莉刘丹宁红
Owner 沈阳万爱普利德医药科技有限公司
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