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Preparation method of high-purity anthocyanin

A technology of high-purity pepperanthin, which is applied in the field of preparation of high-purity pepperanthin, can solve the problems of poor quality, many impurities, and low content of pepperianin, and achieve the effect of large preparation volume, short process and easy to obtain

Active Publication Date: 2015-08-26
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no preparation method for high-purity pianthanin in the market. The pianthanin produced by solvent extraction has low content and poor quality. The prickly ash extract produced by supercritical method contains more impurities, which is not easy to be used in cosmetics and medicines.

Method used

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  • Preparation method of high-purity anthocyanin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Weigh 100 g of Zanthoxylum bungeanum oleoresin produced by a supercritical method with a purity of 50%, add 1 L of mixed solvent (methanol:chloroform=3:7 volume ratio), stir and dissolve at 0°C for 1 hour, extract 3 times in total, and filter through filter paper , the filtrate was concentrated, and the concentrate was dried in a far-infrared box for 1h at a drying temperature of 50°C to obtain 63g of solid matter; 300ml of n-hexane was added to the solid matter, heated and stirred at 45°C for extraction, extracted 3 times, and filtered while hot; the filtrate was Cool with cold water and place for crystallization. After crystallization, immediately crystallize at -5°C for 48 hours, vacuum filter at -5°C to obtain white crystals, wash with n-hexane, and vacuum filter at -5°C. Drying at MPa and 5°C for 5 hours can obtain high-purity ananthocambin crystals. figure 1 As shown, the obtained xanthanin crystals were analyzed by high performance liquid chromatograph...

Embodiment 2

[0018] Example 2: Weigh 150 g of Zanthoxylum bungeanum oleoresin obtained by a supercritical method with a purity of 50%, add 1L of ethanol, stir and dissolve at 5°C for 2 hours, extract 4 times in total, filter through filter paper, concentrate the filtrate, and dry the concentrate in a far-infrared box 1.5h, drying temperature 60°C, to obtain 92g of solid matter; add 500ml of n-hexane to the solid matter, heat and stir at 50°C for extraction, extract 4 times, and quickly filter while hot; the filtrate is cooled with cold water and placed for crystallization, and after the crystals have just precipitated , immediately crystallized at 0°C for 60 hours, vacuum-filtered at -10°C to obtain white crystals, washed with n-hexane, vacuum-filtered at -10°C, and dried for 4 hours at a vacuum degree of 0.095MPa and 5°C to obtain Xanthanin crystals were analyzed by high performance liquid chromatography, and the purity was 91.5%.

[0019] 1 water huiMP purification method, characterized ...

Embodiment 4

[0020] Example 4: Weigh 200 g of Zanthoxylum bungeanum oleoresin obtained by a supercritical method with a purity of 60%, add 1 L of mixed polar solvent of methanol and ethyl acetate with a volume ratio of 1:1, stir and dissolve at -5°C for 1.5 h, and extract 5 Once, filter through filter paper, concentrate the filtrate, and dry the concentrate in a far-infrared box for 0.5h at a drying temperature of 70°C to obtain 140g of solid matter; add 1.4L of n-hexane to the solid matter, heat and stir at 40°C for extraction, and extract 4 times. Heat rapid filtration; the filtrate is cooled and placed for crystallization. After the crystals have just precipitated, immediately crystallize at 5°C for 72 hours, vacuum filter at 0°C to obtain white crystals, then wash with n-hexane, and vacuum filter at 0°C. , and dried at 30°C for 2 hours to obtain the crystals of xanthanin, which was analyzed by high performance liquid chromatography, and the purity was 91.9%.

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Abstract

The invention discloses a preparation method of high-purity sanshoamides. The method comprises the following steps: (1) using pepper oleoresin as a raw material, adding a polar solvent to the pepper oleoresin mixing for extraction, and filtering, concentrating and drying the extraction liquid to obtain solids; (2) adding n-hexane to the solids, heating and stirring for extraction, and filtering to obtain a filtrate; and (3) the cooling, crystallizing and filtering the filtrate to obtain a white crystal; washing the white crystal with hexane, filtering and drying to obtain sanshoamides crystal. The method omits various chromatographic columns, and has short flow and large preparation amount; and the method has characteristics of simpleness, reliability, cost saving, and easiness to obtain the high-purity sanshoamides. The crystal obtained by the method is analyzed by an HPLC column to have a purity higher than 90%, and meets the application requirements of cosmetic and pharmaceutical fields.

Description

technical field [0001] The invention relates to a purification method, in particular to a preparation method of high-purity pepperocannin. Background technique [0002] The chemical components of Zanthoxylum bungeanum mainly include volatile oils, alkaloids, amides, fatty acids, lignans and coumarins, and other components include triterpenes, sterols, hydrocarbons and flavonoid glycosides. The active ingredients in Zanthoxylum bungeanum have the effects of killing insects, inhibiting bacteria, inhibiting platelets, repelling insects, anti-oxidation, and anti-fatigue. Therefore, Zanthoxylum bungeanum has great research and utilization value. [0003] Xanthanin is a series of unsaturated fatty amides, which is an important active ingredient in Zanthoxylum bungeanum, and is also the main component of Zanthoxylum bungeanum. A pharmacological effect. The α-sanshool and β-sanshool in the numbing substance of Zanthoxylum bungeanum can keep the circular muscle of the gastric body ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/09C07C231/24
Inventor 李凤飞杨文江刘素娟
Owner CHENGUANG BIOTECH GRP CO LTD
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