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Method for separating and purifying tripterine from medicinal material celastrus orbiculatus

A technology for the separation and purification of tripterygne, which is applied in the field of separation and purification of tripteryne from the medicinal material of S. chinensis, can solve the problems of complex purification process, insufficient simplification of purification steps, large consumption, etc., and achieve simplified purification steps, purification Easy steps and cost-saving effect

Inactive Publication Date: 2013-08-14
成都彼斯特生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantages are: although the extraction with low-level chloroalkane extracts less impurities, the reagent is highly toxic and consumes a large amount, and the subsequent purification process is also more complicated and the cost is higher
Its defect is: although no toxic reagent is used, but after many times of alkali dissolution and acid precipitation, the product yield will be greatly reduced
Its defect is: the purification step is not simplified enough, the polarity of tripterine is relatively small, if suitable elution conditions are found, qualified products can be obtained, the proportioning of the eluent is not specifically stated in this invention, only the general middle Non-toxic silica gel column, it is not easy to directly collect qualified products during the elution process, and recrystallization is required, resulting in a large loss of products

Method used

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  • Method for separating and purifying tripterine from medicinal material celastrus orbiculatus
  • Method for separating and purifying tripterine from medicinal material celastrus orbiculatus
  • Method for separating and purifying tripterine from medicinal material celastrus orbiculatus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Prepare tripteryglide monomer according to the following steps:

[0033] (1) Material preparation: Crush the above-ground vines and underground roots of S. chinensis into 2-5mm sections.

[0034] (2) Use 90% ethanol to reflux extract the crushed S. serpentine. The ratio of the mass of S. serpentine to the volume of ethanol is 1:10. The units are kilograms and liters respectively. The extraction temperature is 60°C , The extraction time is 5h; the extract is recovered at 60°C under reduced pressure to obtain a concentrated solution.

[0035] (3) Mix the concentrated solution obtained in the above step (2) with 60-80 mesh silica gel at a ratio of 1:1, dry it into dispersed particles, and obtain granular raw materials for later use.

[0036](4) Put 200-300 mesh silica gel in a dichloromethane-methanol solution with a volume ratio of 25:1 for wet packing. The diameter of the separation column is 15 cm, and use a dichloromethane-methanol solution with a volume ratio of 25:1...

Embodiment 2

[0039] Prepare tripteryglide monomer according to the following steps:

[0040] (1) Material preparation: Crush the above-ground vines and underground roots of S. chinensis into 2-5mm sections.

[0041] (2) Use 92% ethanol to reflux extract the crushed Snakevine segment. The ratio of the mass of S. Schidenia to the volume of ethanol is 1:15, and the units are kilograms and liters respectively. The extraction temperature is 65°C , The extraction time is 6h; the extract is recovered at 62°C under reduced pressure to obtain a concentrated solution.

[0042] (3) Mix the concentrated solution obtained in the above step (2) with 60-80 mesh silica gel at a ratio of 1:1, dry it into dispersed particles, and obtain granular raw materials for later use.

[0043] (4) Put 200-300 mesh silica gel in a dichloromethane-methanol solution with a volume ratio of 22:1 for wet packing. The diameter of the separation column is 18 cm, and use a dichloromethane-methanol solution with a volume ratio...

Embodiment 3

[0046] Prepare tripteryglide monomer according to the following steps:

[0047] (1) Material preparation: Crush the above-ground vines and underground roots of S. chinensis into 2-5mm sections.

[0048] (2) Use 95% ethanol to reflux extract the crushed S. serpentine. The ratio of the mass of S. serpentine to the volume of ethanol is 1:20. The units are kilograms and liters respectively. The extraction temperature is 70°C , The extraction time is 7h; the extract is recovered at 65°C under reduced pressure to obtain a concentrated solution.

[0049] (3) Mix the concentrated solution obtained in the above step (2) with 60-80 mesh silica gel at a ratio of 1:1, dry it into dispersed particles, and obtain granular raw materials for later use.

[0050] (4) Put 200-300 mesh silica gel in a dichloromethane-methanol solution with a volume ratio of 20:1 for wet packing. The diameter of the separation column is 20 cm, and use a dichloromethane-methanol solution with a volume ratio of 20:...

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Abstract

The invention discloses a method for separating and purifying tripterine from a medicinal material celastrus orbiculatus, which comprises the following steps: (1) acquiring a concentrated solution from the medicinal material celastrus orbiculatus, stirring with silica gel, and drying into dispersed granules to obtain the granular raw material for later use; (2) adding silica gel in a dichloromethane-methanol solution, packing by a wet process, and balancing the separation column with the dichloromethane-methanol solution; after well balancing, feeding the granular raw material; carrying out gradient elution with an eluting agent, wherein the eluting agent is composed of a dichloromethane-methanol solution and ammonia water, and a small amount of anhydrous sodium sulfate is also added into the eluting agent with remove water in the eluting agent; collecting the eluate to obtain a tripterine crude solution; recovering the eluting agent under reduced pressure to obtain a tripterine pure product; and washing the tripterine pure product with methanol or anhydrous ethanol to obtain the tripterine monomer. By using the dichloromethane-methanol solution and ammonia water for elution, the invention has the advantages of simple technique, high efficiency, environment friendliness, high yield and high production rate, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for extracting tripterygne from S. chinensis, in particular to a method for separating and purifying tripterygne from S. sulphae. Background technique [0002] Tripteryglide, also known as celastrol and celastrol, belongs to triterpenoids, its molecular formula is C29H38O4, its molecular weight is 450.61, and its structural formula is as follows: [0003] [0004] Tripterygium wilfordii is stable in nature and is one of the main active ingredients in Snakevine and Tripterygium wilfordii. It mainly exists in the root bark and has anti-oxidation, anti-inflammation, anti-virus, anti-fertility, anti-senile dementia, and anti-tumor activities. activity and regulation of autoimmunity. The current reports on tripterygium mainly focus on the study of the traditional Chinese medicine Tripterygium wilfordii, and the main research site is the root bark. [0005] There are many traditional tripterine extraction methods, but a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 董维珍常建红王小琴冉波
Owner 成都彼斯特生物科技有限公司
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