Gambogic acid separating and purifying production process

A separation, purification and production process technology, applied in the field of extraction, separation and purification of natural products, can solve the problems of low purity, long existence cycle and low yield, and achieve the effects of simple process flow, low cost and high yield

Inactive Publication Date: 2012-07-25
PI & PI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many methods for extraction and preparation. Garcinia is the colloidal resin of the plant Garcinia cambogia. It becomes a block after drying and must be crushed before it can be fully extracted. Gambogic acid esters have strong solubility, and most of them can be removed by extraction with a low-polarity solvent. Impurities are convenient for subsequent separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0010] 1. Grinding: Take 10g of Garcinia Cambogia and grind it to 400-500 mesh with a high-speed grinder.

[0011] 2. Extraction: reflux the crushed garcinia cambogia with 100g ethyl acetate twice, each time for 1h, filter, recover, and mix the sample with 12g silica gel.

[0012] 3. Medium-pressure silica gel column separation: dry-pack the mixed 12g silica gel column, the column volume is 500ml, the sample volume is 1 / 6 of the separation silica gel, first moisten the column with 500ml petroleum ether, and the flow rate is controlled at 1 / 6BV / min, then isocratic elution with petroleum ether: ethyl acetate = 9:1, and 95% gambogic acid was obtained by fraction collection.

[0013] 4. ODS purification: Dissolve 95% gambogic acid in DMSO, put it on a medium-pressure ODS column, elute with 85% methanol, and control the flow rate at 1 / 6BV / min to obtain more than 99% gambogic acid.

Embodiment approach 2

[0015] 1. Grinding: Take 100g of Garcinia Cambogia and grind it to 400-500 mesh with a high-speed grinder.

[0016] 2. Extraction: reflux the pulverized garcinia cambogia twice with 1000g ethyl acetate, 1 hour each time, filter, recover, and mix the sample with 120g times silica gel.

[0017] 3. Medium-pressure silica gel column separation: dry-pack the mixed 120g silica gel column, the column volume is 5L, the sample volume is 1 / 6 of the separation silica gel, 5L is moistened with petroleum ether, and the flow rate is controlled at 1 / 6BV / min Then use petroleum ether:ethyl acetate=9:1 isocratic elution, when the elution reaches 3BV, collect according to fractions to obtain 95% gambogic acid.

[0018] 4. ODS refinement: Dissolve 95% gambogic acid in DMSO, apply medium-pressure ODS, elute with 85% methanol, and control the flow rate at 1 / 6BV / min to obtain more than 99% gambogic acid.

Embodiment approach 3

[0020] 1. Grinding: take 1kg of gamboge, and grind it to 400-500 mesh with a high-speed grinder.

[0021] 2. Extraction: reflux the crushed garcinia cambogia twice with 10kg of ethyl acetate, 1 hour each time, filter, recover, and mix with 1.2kg of silica gel.

[0022] 3. Medium-pressure silica gel column separation: dry-pack the mixed 1.2kg silica gel column, the column volume is 50L, the sample volume is 1 / 6 of the separation silica gel, moisten the column with 50L petroleum ether, and the flow rate is controlled at 1 / 6BV / min and then eluted isocratically with petroleum ether: ethyl acetate = 9:1. When washing 3BV, 95% gambogic acid was obtained by collecting fractions.

[0023] 4. ODS purification: Dissolve 95% gambogic acid in DMSO, put it on a medium-pressure ODS column, elute with 85% methanol, and control the flow rate at 1 / 6BV / min to obtain more than 99% gambogic acid.

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PUM

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Abstract

The invention relates to a gambogic acid separating and purifying production process, which includes crushing, extracting, medium-pressure silicagel column chromatography and ODS (octadecyl silane) refining. The process is simple in procedure, low in cost, short in cycle and high in yield, gambogic acid purity is up to more than 99%, and the process is suitable for large-scale industrial preparation of high-purity gambogic acid. The gambogic acid needs to be well ground to facilitate better extraction, and most high-polarity impurities can be quickly removed by extraction. Column efficiency is higher and separation degree is higher by means of 300-400-mesh silicagel chromatographic separation at medium pressure, and purity can reach more than 99% after ODS refining.

Description

technical field [0001] The patent of the invention relates to a method for preparing high-purity gambogic acid from gambogic, which belongs to the field of extraction, separation and purification of natural products, and related technologies such as extraction, extraction, silica gel column separation and fine fractionation. Background technique [0002] Gambogic acid is the main anti-cancer active ingredient in gamboge, with the highest content. There are many methods for extraction and preparation. Garcinia is the colloidal resin of the plant Garcinia cambogia. It becomes a block after drying and must be crushed before it can be fully extracted. Gambogic acid esters have strong solubility, and most of them can be removed by extraction with a low-polarity solvent. Impurities are convenient for subsequent separation and purification. Traditionally, there is recrystallization after salt formation. Not only the yield is low but the purity is not high. Normal pressure silica ge...

Claims

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Application Information

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IPC IPC(8): C07D493/20
Inventor 袁晓周东斌林顺权
Owner PI & PI BIOTECH
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