Method for separating and purifying malvidin glucoside from grape-skin red

A technology for malvain and glucoside, which is applied in the field of separation and purification of high-purity malvain glucoside, can solve the problems of large amount of filler, high price and high production cost, and achieves the effects of large separation capacity, low cost and low cost

Active Publication Date: 2014-06-18
XIAN RUILIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Preparative chromatography uses a large amount of filler and is expensive, resulting in high production costs

Method used

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  • Method for separating and purifying malvidin glucoside from grape-skin red

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) After dissolving 500.0g of grape skin red with 5L of water completely, put it on the D101 macroporous adsorption resin column through treatment, and use the collected eluent to rinse the column repeatedly to make it fully adsorbed, then use pH 3 water and The volume percentage is the gradient elution of 20%, 40%, 60%, 80% and 95% ethanol aqueous solution, and every 1L is used as a receiving volume, detected by HPLC, and the components rich in malvalin glucoside are combined, and the Concentrate under reduced pressure at a temperature of ≤70°C and a vacuum of 0.05-0.08 MPa to obtain 3.1 g of crude product I, with a malvalin glucoside content of 21.8%.

[0027] (2) After mixing 250.0 g of activated carbon and 250.0 g of diatomaceous earth evenly, soak in chloroform for 30 minutes, and wet-pack the column with a diameter-to-height ratio of 1:8. Get the crude product I (the average content of malvalin glucoside is 22.3%) 50.0g obtained by macroporous adsorption resin en...

Embodiment 2

[0032] (1) After dissolving 500.0g of grape skin red with 5L of water completely, put it on the D201 macroporous adsorption resin column after treatment, and use the collected eluent to rinse the column repeatedly to make it fully adsorbed, then use pH 4 water and The volume percentage is 15%, 30%, 45%, 60%, 75% and 95% ethanol aqueous solution gradient elution, each 1L is used as a receiving volume, detected by HPLC, and the components rich in malvalin glucoside are combined, Concentrate it under reduced pressure at a temperature of ≤70°C and a vacuum of 0.05-0.08 MPa to obtain 2.8 g of crude product I, with a malvalin glucoside content of 23.2%.

[0033] (2) After mixing 250.0 g of activated carbon and 250.0 g of diatomaceous earth evenly, soak in chloroform for 30 minutes, and wet-pack the column with a diameter-to-height ratio of 1:4. Get the crude product I (the average content of malvalin glucoside is 24.1%) 50.0g that macroporous adsorption resin enrichment obtains and ...

Embodiment 3

[0038] (1) After completely dissolving 500.0g grape skin red with 5L water, put it on the treated Diaion HP-20 macroporous adsorption resin column, and wash the column repeatedly with the collected eluent to make it fully adsorbed, then use a pH value of 5 Gradient elution of water and 20%, 40%, 60%, 80% and 95% ethanol aqueous solution by volume percentage, each 1L is regarded as a receiving volume, detected by HPLC, and the components rich in malvalin glucoside are combined , concentrated under reduced pressure at a temperature of ≤70° C. and a vacuum of 0.05 to 0.08 MPa to obtain 4.1 g of crude product I, with a malvalin glucoside content of 21.9%.

[0039] (2) After mixing 250.0 g of activated carbon and 250.0 g of diatomaceous earth evenly, soak in chloroform for 30 minutes, and wet-pack the column with a diameter-to-height ratio of 1:8. Get the crude product I (the average content of malvalin glucoside is 26.4%) 50.0g obtained by macroporous adsorption resin enrichment a...

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Abstract

The invention relates to a method for separating and purifying malvidin glucoside from grape-skin red, which has the following advantages that: products are high in purity and low in cost; raw materials are easily available and are free of pollution; and used equipment is simple and is suitable for industrial production. The method comprises the following steps of: processing grape-skin red after dissolved with water by a macroporous adsorbent resin chromatographic column, carrying out gradient elution by using an aqueous and / or alcoholic solution, collecting components containing the malvidin glucoside, and carrying out pressurized concentration to obtain a crude product I; processing the crude product I by an activated carbon and diatomite mixed chromatographic column, eluting by using a chloroform and alcohol solution, and carrying out heating and reduced-pressure concentrating on eluent to obtain a crude product II; and processing the crude product II by a polyamide chromatographic column, carrying out gradient elution by using an aqueous and / or alcoholic solution, combining components with similar contents, repeatedly processing the combined components by the polyamide chromatographic column to obtain the malvidin glucoside with the content of 95%, and recrystallizing repeatedly through butanone-alcohol to obtain the malvidin glucoside with the content of more than 98%.

Description

technical field [0001] The invention belongs to the field of natural medicine extraction, in particular to a method for separating and purifying high-purity malvalin glucoside from grape skin red. Background technique [0002] Grape skin red is obtained by removing seeds and sundries from the residue after making grape juice or wine, and refining it through extraction, filtration, concentration, etc. It belongs to anthocyanin pigments. Anthocyanins belong to flavonoids, which have the functions of anti-inflammation, improving immunity, anti-oxidation, eliminating free radicals, improving lipids in the liver and serum, preventing arteriosclerosis, and improving vision. [0003] Malvidin-3-O-glucoside (malvidin-3-O-glucoside) is a flavonoid component with flavonoid as the mother core, and its structural formula is as follows: [0004] [0005] The compound has high polarity, good water solubility, is easily soluble in methanol and ethanol, and insoluble in non-polar solven...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/065C07H1/08
Inventor 李启贵冯震邓师勇冯小琼高晨强婷华高仁孝
Owner XIAN RUILIAN NEW MATERIAL CO LTD
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