Limonin analogue and separation and purification method thereof

A technology for the separation and purification of limonin, which is applied in the fields of organic chemistry and steroids, and can solve the problems of less research on the purification route of limonin analogues

Inactive Publication Date: 2012-09-12
CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few studies on the purification route of limonoid analogues in orange core

Method used

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  • Limonin analogue and separation and purification method thereof
  • Limonin analogue and separation and purification method thereof
  • Limonin analogue and separation and purification method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0025] 1. Preparation of Sample Solution

[0026] Method 1: Weigh a certain amount of orange stone powder, add petroleum ether (boiling point 60 ℃ ~ 90 ℃), reflux and degrease in a water bath at 50 ~ 60 ℃ for 4 ~ 6 hours, after discarding the petroleum ether, press 1:6 ~ 1:10 Add 40-50% ethanol to the solid-liquid ratio, reflux and extract in a water bath at 50-60°C for 1-2 hours, filter with suction, concentrate the filtrate, and set aside.

[0027] Method 2: Weigh a certain amount of tangerine peel powder, add 40-50% ethanol at a solid-liquid ratio of 1:6-1:10, ultrasonically extract for 1-2 hours, filter with suction, concentrate the filtrate, and set aside.

[0028] Method 1 is mainly for medicinal materials with high fatty oil content in the seeds of citrus plants of Rutaceae, such as orange core and pomelo core; method 2 is mainly for medicinal materials with low fatty oil content in other parts of citrus plants in Rutaceae, such as tangerine peel and citrus aurantium. ...

preparation example 1

[0073] 1) Take a few grams of orange core, crush it, add petroleum ether (boiling point 60°C-90°C) to reflux for degreasing, the temperature of the water bath is 50-60°C, and the degreasing time is 6h; the reflux condition is: 50% ethanol is the weight of the orange core powder 10 times of that, the extraction temperature is 50~60°C, and the extraction time is 2h. Filter to obtain the extract;

[0074] 2) The extract was purified by HPD-722 macroporous resin column chromatography through three steps of sample loading, adsorption and elution, and the eluate was collected and dried to obtain the purified sample.

[0075] Among them: sample loading: the extract is prepared into a sample solution with a concentration of 4.5 mg / mL, the pH of the sample solution is controlled within the range of 6.0 to 7.0, and the sample is loaded at a flow rate of 1.0 to 2.0 BV / h;

[0076] Adsorption: After loading the sample, let it stand for more than 30 minutes for adsorption, and wash it with...

preparation example 2

[0080] 1) Take the medicinal material of Fructus Fructus Fructus and heat it to reflux for extraction. The reflux conditions are: 50% ethanol is 6 times the weight of Fructus Fructus Fructus powder, the extraction temperature is 50-60°C, and the extraction time is 2 hours. Filter to obtain the extract;

[0081] 2) The extract was purified by HPD-722 macroporous resin column chromatography through three steps of sample loading, adsorption and elution, and the eluate was collected and dried to obtain the purified sample.

[0082] Among them: sample loading: the extract is prepared into a sample solution with a concentration of 5.5 mg / mL, the pH of the sample solution is controlled within the range of 6.0 to 7.0, and the sample is loaded at a flow rate of 1.0 to 2.0 BV / h;

[0083] Adsorption: After loading the sample, let it stand for more than 30 minutes for adsorption, and wash it with 1.0BV of distilled aqueous solution;

[0084] Elution: After washing, use 80-90% ethanol sol...

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Abstract

The invention belongs to the field of the extraction of natural medicines and particularly relates to a limonin analogue and a separation and purification method thereof. The invention aims to solve the technical problem of providing a fire-new separation and purification method of a limonin analogue. According to the separation and purification method disclosed by the invention, the medicinal materials of rue family citrus plants, such as tangerine seeds, pummelo seeds, immature bitter oranges, tangerine peels and the like, are used as raw materials, 40 to 50 percent of ethanol is used as a solvent for extraction, an extract is separated and purified by adopting HPD-722 type macroporous resin, the content of the limonin analogue in obtained solid matters is greater than 80 percent, the content of limonin is greater than 20 percent, and the content of nomilin is greater than 40 percent. The method has high extraction efficiency, little reagent consumption and little pollution and is simple to operate.

Description

technical field [0001] The invention belongs to the field of natural medicine extraction, and specifically relates to a separation and purification method for obtaining limonoid analogues from Rutaceae citrus medicinal materials such as tangerine core, pomelo core, orange core, citrus aurantium, tangerine peel, and aurantia citrus as raw materials. Background technique [0002] Limonoid analogues are a class of highly oxidized tetracyclic triterpenoid plant secondary metabolites, which widely exist in Rutaceae and Meliaceae plants. Among limonoid analogues, limonin and nomilin have higher content, which have anti-cancer, analgesic, anti-inflammatory, anti-anxiety, prevent atherosclerotic formation, enhance antioxidant capacity and antibacterial effects. [0003] Orange pit is the dry mature seed of Citrus reticulate Blanco and its cultivars of Rutaceae plant. Limonin analogues are the main effective components of orange pit, which mainly exist in the alcohol-soluble extracti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
Inventor 裴瑾万德光何中燕周明眉莫书蓉
Owner CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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