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Method for separating and purifying barbaloin through preparative high performance liquid chromatography

A kind of technology of aloin and aloin crude product, which is applied in the direction of organic chemistry, etc.

Inactive Publication Date: 2014-05-14
江苏汉邦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the technology of separating various monomers in aloe is still immature, and most of the aloe products used are the mixture of aloe extracts. If the active ingredients in aloe can be preparatively separated, it can be used in medicines and health products, especially for the medical industry. It will be a very favorable development direction. Therefore, it will be a great progress in natural medicine research to establish a method and technology for extracting, separating and purifying aloin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0014] 1. Extraction: After sieving the powder, weigh 80g and place it in an extractor, extract with 1000mL of 50% ethanol, reflux in a water bath at 70°C for 1 hour, extract once, combine the extracts, and concentrate under reduced pressure to form a paste;

[0015] 2. Dissolution of samples: Dissolve the concentrate in mobile phase with a concentration of 10g / mL, filter and set aside;

[0016] 3. Preparation of mobile phase: mobile phase is methanol: water = 42:58;

[0017] 4. DAC column separation: use a sampling pump to pump the sample solution into the dynamic axial compression column (50*500mm) filled with a particle size of 20um, the injection flow rate is 60mL / min, and elute with the mobile phase. The flow rate is 100mL / min, collect the target components, and sample for HPLC detection;

[0018] 5. Concentration: Concentrate the collected target components to obtain pure aloin, which is 98.6% pure by HPLC.

[0019]

Embodiment approach 2

[0021] 1. Extraction: After sieving the powder, weigh 100g and place it in an extractor, extract with 1200mL of 50% ethanol, reflux in a water bath at 70°C for 1 hour, extract twice, combine the extracts, and concentrate under reduced pressure to form a paste;

[0022] 2. Dissolution of samples: Dissolve the concentrate in mobile phase with a concentration of 15g / mL, filter and set aside;

[0023] 3. Preparation of mobile phase: mobile phase is methanol: water = 45:55;

[0024] 4. DAC column separation: use a sampling pump to pump the sample solution into the dynamic axial compression column (50*500mm) filled with a particle size of 20um, the injection flow rate is 60mL / min, and elute with the mobile phase. The flow rate is 80mL / min, collect the target components, and sample for HPLC detection;

[0025] 5. Concentration: Concentrate the collected target components to obtain pure aloin, which is 98.8% pure by HPLC.

[0026]

Embodiment approach 3

[0028] 1. Extraction: After sieving the powder, weigh 150g and place it in an extractor, extract with 1800mL of 50% ethanol, reflux in a water bath at 70°C for 1 hour, extract twice, combine the extracts, and concentrate under reduced pressure to form a paste;

[0029] 2. Dissolution of samples: Dissolve the concentrate in mobile phase with a concentration of 20g / mL, filter and set aside;

[0030] 3. Preparation of mobile phase: mobile phase is methanol: water = 44:56;

[0031] 4. DAC column separation: use a sampling pump to pump the sample solution into the dynamic axial compression column (50*500mm) filled with a particle size of 20um, the injection flow rate is 60mL / min, and elute with the mobile phase. The flow rate is 80mL / min, collect the target components, and sample for HPLC detection;

[0032] 5. Concentration: Concentrate the collected target components to obtain pure aloin, the purity of which is 98.5% as detected by HPLC.

[0033]

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Abstract

The invention relates to a method for purifying a natural product, and concretely relates to a method for preparing highly pure barbaloin, and a technology thereof. Barbaloin is separated and purified through the method adopting ethanol to realize heating refluxing extraction, reverse phase silica gel as a DAC preparative column filler and a mixed solvent containing methanol and water as a mobile phase. The separation technology has the advantages of simplicity, high extraction rate, high product purity and no pollution, and is suitable for separating and preparing barbaloin.

Description

technical field [0001] The invention relates to a method for separating and purifying aloin with a dynamic axial compression column, specifically a method for separating and purifying aloin by heating and reflux extraction and a dynamic axial compression preparation column. Background technique [0002] Aloe vera is a perennial succulent herb of Liliaceae. Modern pharmacological experiments have proved that aloe vera has many pharmacological effects such as healing, purging, inhibiting and killing bacteria, anti-inflammatory, anti-tumor, anti-virus, anti-aging, lowering blood sugar, lowering blood fat, and strengthening the heart. The main natural active ingredient contained in aloe vera is aloin, which is an anthraquinone compound. At present, the technology of separating various monomers in aloe is still immature, and most of the aloe products used are the mixture of aloe extracts. If the active ingredients in aloe can be preparatively separated, it can be used in med...

Claims

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Application Information

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IPC IPC(8): C07D309/10
CPCC07D309/10
Inventor 张大兵张宁罗军侠刘玉明王亚辉
Owner 江苏汉邦科技股份有限公司
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