Method for extracting oligomeric proanthocyanidins

A technology of oligomeric proanthocyanidins and extracts, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve problems such as high cost, unsatisfactory product purity and yield, cumbersome operation, etc., and achieve low cost , improved purity and yield, and simple process

Inactive Publication Date: 2010-09-29
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome defects such as unsatisfactory product purity and yield of existing oligomeric proanthocyanidins, or cumbersome operation, or high cost, and

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1) Weigh 250g seabuckthorn seeds (produced in Qinghai), add 600ml of 60% ethanol aqueous solution, stir and extract, and the extraction temperature is controlled at 40°C. The first extraction time was 60 minutes, the second and third extraction times were 20 minutes respectively, and a total of three extractions were performed. Filtrate after each extraction, combine the filtrates, and concentrate to obtain a concentrated solution of oligomeric proanthocyanidins. The content of oligomeric proanthocyanidins accounted for 57.6wt% of the solid content of the concentrated liquid. In this step, the yield of oligomeric proanthocyanidins is 92.7%.

[0039] 2) The size of the chromatographic column is φ12×500mm, and the interior is filled with D101 macroporous adsorption resin (50 times the mass of the sample). In the following operations, the temperature was controlled at 30°C. The oligomeric proanthocyanidin concentrate is passed into the chromatography column at a flow ra...

Embodiment 2

[0043] 1) Weigh 250g seabuckthorn seeds (produced in Qinghai), add 800ml of 70% methanol aqueous solution, and reflux extraction, the extraction temperature is controlled at 85°C. The first extraction time was 30 min, the second and third extraction time were 15 min respectively, and a total of three extractions were performed. Filtrate after each extraction, combine the filtrates, and concentrate to obtain a concentrated solution of oligomeric proanthocyanidins. The content of oligomeric proanthocyanidins accounted for 38.8wt% of the solid content of the concentrated liquid. In this step, the yield of oligomeric proanthocyanidins is 89.1%.

[0044] 2) The size of the chromatographic column is φ12×500mm, and the interior is filled with AB-8 macroporous adsorption resin (80 times the mass of the sample). In the following operations, the temperature was controlled at 30°C. The oligomeric proanthocyanidin concentrate is passed into the chromatography column at a flow rate of 0...

Embodiment 3

[0048] 1) Weigh 250g seabuckthorn seeds (produced in Qinghai), add 1000ml of 70% acetone-water solution, and perform ultrasonic extraction, and the extraction temperature is controlled at 30°C. The first extraction time was 90 min, the second and third extraction time were 60 min respectively, and a total of three extractions were performed. Filtrate after each extraction, combine the filtrates, and concentrate to obtain a concentrated solution of oligomeric proanthocyanidins. The content of oligomeric proanthocyanidins accounts for 47.5% by weight of the solid content of the concentrated liquid. In this step, the yield of oligomeric proanthocyanidins is 91.1%.

[0049] 2) The size of the chromatographic column is φ50×500mm, and the interior is filled with HP-20 macroporous adsorption resin (100 times the mass of the sample). In the following operations, the temperature was controlled at 25°C. The oligomeric proanthocyanidin concentrate is passed into the chromatography col...

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Abstract

The invention discloses a method for extracting oligomeric proanthocyanidins, which comprises the following steps of: extracting a plant raw material containing the oligomeric proanthocyanidins with a solvent; enabling a crude extract to pass through a macroporous adsorbent resin column; eluting with water to remove protein and polysaccharide impurities; carrying out gradient elution with water and one or more selecting from alcohol, methyl alcohol and acetone as an eluant; collecting mixed solution with the volume ratio of n-butyl alcohol, acetic acid and water of 4:1:5; standing for demixing, wherein the solution at upper layer is a developing solvent; and carrying out silica gel thin-layer chromatography, wherein the elution part with the Rf value of 0.2-0.5 on a thin-layer chromatography plate is the oligomeric proanthocyanidins extract. Compared with the prior art, the invention has the advantages that the purity and the yield are both remarkably improved, the yield of the oligomeric proanthocyanidins can reach more than 80 percent, the product purity is no less than 50 percent and is basically more than 80 percent, and the method has simple and convenient process, low cost and easy industrialization.

Description

technical field [0001] The invention relates to an extraction method, in particular to an extraction method of oligomeric proanthocyanidins. Background technique [0002] Proanthocyanidins (PC), widely present in plants, are a class of polyphenolic substances condensed from different amounts of flavan-3-ol monomers, mainly composed of catechin and epicatechin, etc. Composition, which is named after the corresponding anthocyanin is formed by heating in an acidic medium. The simplest proanthocyanidins are catechin and epicatechin monomers. In addition, there are dimers, trimers, tetramers, etc., up to decamers. According to the degree of polymerization, 2- to 4-mers are usually called oligomers (oligomeric procyanidin, OPC), and pentamers and above are called polymeric procyanidins (PPC). Oligomeric procyanidins (OPCs) have become a research hotspot because of their special structure, good water solubility, high effectiveness, and bioavailability above 90%. They are easily ...

Claims

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Application Information

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IPC IPC(8): C07D311/62B01D15/34B01J20/26
CPCY02P20/54
Inventor 高雯夏玉叶闵旸王曙光盖春艳韩竹箴陈述增
Owner SHANGHAI INST OF PHARMA IND
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