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Chemical complexing directional separation and purification method for preparing high-purity beta-elemene raw material medicament

A technology for directional separation and elemene, applied in distillation purification/separation, adsorption purification/separation, hydrocarbon purification/separation, etc., can solve the problems of poor extraction stability of instruments and equipment, complicated production equipment, expensive cost, etc., and achieve production Efficiency improvement, simple equipment and high yield

Inactive Publication Date: 2009-09-16
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

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Problems solved by technology

[0008] The purpose of the present invention is to provide a low-content 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 as a starting material

Method used

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  • Chemical complexing directional separation and purification method for preparing high-purity beta-elemene raw material medicament
  • Chemical complexing directional separation and purification method for preparing high-purity beta-elemene raw material medicament

Examples

Experimental program
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Effect test

Embodiment 1

[0020] a. using steam distillation to extract volatile oil from zedoary tubers, wherein the content of β-elemene is 8.1%, and the volatile oil of 100g is taken as raw material;

[0021] b. After freezing and filtering the above raw materials in a refrigerator at -4°C, mix the remaining oil phase with 100g of 100-200 mesh silica gel, use a wet method to pack the column, and put the mixed sample on a 1000g 200-300 mesh silica gel column Above, elute with petroleum ether (60-90°C), collect the fractions with low polarity, and use GC or HPLC to detect, it is found that the components with high polarity are basically removed, and the content of β-elemene is 68.2%;

[0022] c. the 68.2% β-elemene obtained in step b is extracted three times with an aqueous solution of 1.0 mol / L silver nitrate with an equal volume concentration, the liquid separation takes the lower layer of water, continues to extract three times with an equal volume of n-hexane, and the upper layer n-hexane The alka...

Embodiment 2

[0025] a. Take the fresh leaves of Lemongrass citronella as a raw material, steam distill it to obtain Java volatile oil, continue vacuum distillation to obtain β-elemene with a content of 16.5%, and take 800g as a raw material.

[0026] b. Mix the above raw materials with 1500g of 100-200 mesh silica gel, use wet method to load the column, put the mixed sample on 15000g of 200-300 mesh silica gel column, elute with cyclohexane, and collect The fractions were detected by GC or HPLC, and it was found that the components with large polarity were basically removed, and the content of β-elemene was 70.5%.

[0027] c, the 70.5% beta-elemene obtained in step b is extracted three times with an aqueous solution of 1.8mol / L silver nitrate with an equal volume concentration, and the lower layer of the aqueous phase is taken by liquid separation, and continues to be extracted three times with an equal volume of n-hexane, and the upper layer n-hexane The alkane was concentrated under redu...

Embodiment 3

[0030] a. Take the fresh leaves of Solidago sativa as raw material, extract it with carbon dioxide supercritical fluid to obtain the volatile oil of Solidago sativa, wherein the content of β-elemene is 14.3%, and after continuous distillation, β-elemene with a content of 40.6% is obtained Alkene, take 500g as raw material.

[0031]b. Mix the above raw materials with 800g of 100-200 mesh silica gel, and use the wet method to load the column. Put the mixed sample on the 8000g of 200-300 mesh silica gel column, elute with petroleum ether, and collect the samples with low polarity. GC or HPLC detection found that some components with high polarity were not removed; the components containing β-elemene were collected and passed through the silica gel column again, and the components with high polarity detected by GC or HPLC were completely removed. The content of β-elemene is 85.6%.

[0032] c, the 85.6% beta-elemene obtained in step b is extracted three times with an aqueous solut...

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Abstract

The invention provides a method for preparing high-purity beta-elemene from a low-content (over 1 percent) elemene raw material, which simplifies the steps of process operation, improves the production efficiency from an initial raw material to the high-purity beta-elemene, and reduces production cost. Compared with the prior art, the method comprises the following main different points: volatile oil constituents with large polarity is removed from the elemene raw material with the content over 1 percent under the action of silica gel column chromatography; then impurity constituents with small polarity is removed form a residual oil phase by a silver nitrate complexation extraction method and silver nitrate bonded silica gel column chromatography; and finally the beta-elemene with the content of between 95.0 and 99.9 percent is obtained through distillation under reduced pressure or rectification. The raw material medicament can be produced into oral administration preparations such as oral emulsions, capsules and the like, and can also be produced into non-intestinal administration preparations such as emulsion injections, water injections, cutaneous permeable agents, lung spray formulations, suppositories and the like. The experimental method has novel design and concise operating steps, obviously improves the yield, and reduces production cost.

Description

Technical field: [0001] The invention relates to a chemical complexation directional separation and purification method for preparing high-purity β-elemene bulk medicine. Background technique: [0002] Elemene is isolated from zedoary oil and citronella oil, and has been widely used to treat cancer. The earliest anticancer drug was zedoary oil injection made from zedoary oil, which can only be used locally The treatment of cervical cancer by tumor drug administration has a long course of treatment and inconvenient administration operation, while other various cancers cannot be effectively treated with this injection. In order to solve the problem of the limitation of the use of zedoary oil injection, people have separated elemene with fixed proportioning components from zedoary oil and citronella oil to make elemene injection. In addition to local tumor administration and regional administration, the milk injection can also be injected intravenously, and can treat cervical ...

Claims

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Application Information

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IPC IPC(8): C07C13/19C07C7/152C07C7/12C07C7/04A61K31/015A61K36/899A61P35/00A61P35/02
CPCC07C7/12A61P35/00A61P35/02C07C13/19
Inventor 孙敏鸽李淑斌
Owner 沈阳万爱普利德医药科技有限公司
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