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Symplocos paniculata fruit compound high-speed countercurrent chromatography preparation method

A high-speed countercurrent chromatography and compound technology, which is applied in the field of high-speed countercurrent chromatography preparation of white sandalwood compounds, can solve the problems of no purification and identification of anthocyanins and flavonoids, no specific structure exploration of compounds, and no disclosure, so as to save separation Cost, low cost, time-saving effect

Active Publication Date: 2018-02-16
张良波
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although, red sandalwood pulp red pigment and white sandalwood leaf total flavonoids have been found in the prior art, and wherein the red pigment belongs to anthocyanins, but there is no purification and identification of anthocyanins and flavonoids from white sandalwood fruit, there is no The specific structure of the compound is investigated
Moreover, there is no disclosure in the prior art that high-purity delphinidin-3-O-seradioside, rutin, quercetin-3-O-glucose are separated from white sandalwood fruit by high-speed countercurrent chromatography (HSCCC). Quercetin-3-O-rhamnoside

Method used

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  • Symplocos paniculata fruit compound high-speed countercurrent chromatography preparation method
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  • Symplocos paniculata fruit compound high-speed countercurrent chromatography preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0066] Determine the solvent system for the separation of anthocyanins by high-speed countercurrent chromatography, prepare a number of solvent systems with different ratios, perform characterization and analysis on them, and calculate the K value of the system. The results are shown in Table 1. It can be seen from Table 1 that the K value of system 5 is reasonable and can be used as a solvent system for high-speed countercurrent chromatography separation. When the sample amount is 60mg, the separation effect of the sample is good, but the separation efficiency is low; Relatively high.

[0067] Table 1

[0068]

[0069]

[0070] Determine the solvent system for the separation of flavonoids by high-speed countercurrent chromatography, analyze and calculate the K value of each component in multiple solvent systems with different ratios, and calculate the degree of separation. The results are shown in Table 2. The K values ​​of the three target components are quite differ...

Embodiment 2

[0074] A kind of sandalwood fruit compound high-speed counter-current chromatography preparation method, is characterized in that, comprises the steps:

[0075] (1) Preparation of extract

[0076] ① Weigh 1.0Kg of white sandalwood fresh fruit, mash it for later use, measure 5L of ethanol with a mass concentration of 40% as the extractant, and set it aside;

[0077] ② Add the crushed white sandalwood fresh fruit to the extractant, ultrasonically extract in the dark for 20 minutes, stir in time, and filter; it is beneficial for the active ingredients in the white sandalwood fruit to enter the extract, and the dark extraction can avoid the light on the active ingredients. have an impact;

[0078] ③ Take the filter residue obtained from the above filtration, and repeat the leaching process of the above steps ① and ② once, so that the active ingredients in the filter residue can enter the extract;

[0079] ④ Combine the above-mentioned filtrates to obtain the crude extract of whi...

Embodiment 3

[0103] A kind of sandalwood fruit compound high-speed counter-current chromatography preparation method, is characterized in that, comprises the steps:

[0104] (1) Preparation of extract:

[0105] ①Weigh 2.0Kg of fresh white sandalwood fruit, mash it for later use, measure 10L of 70% methanol aqueous solution for later use;

[0106] ② Add the crushed white sandalwood fruit to the extractant, ultrasonically extract in the dark for 40 minutes, stir in time, and filter, so that the active ingredients in the white sandalwood fruit will enter the extract, and the active ingredients will not lose their activity;

[0107] ③ Take the filter residue obtained by the above-mentioned filtration, repeat the extraction process of the above-mentioned steps ① and ② twice, so that the active ingredients in the fresh white sandalwood fruit can fully enter the extract;

[0108] ④ Combine the above-mentioned filtrates to obtain the crude extract of white sandalwood fruit.

[0109] (2) Concentr...

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Abstract

The invention discloses a symplocos paniculata fruit compound high-speed countercurrent chromatography preparation method which comprises steps of extract preparation, concentration, primary purification, symplocos paniculata fruit anthocyanin separation, symplocos paniculata fruit flavone separation, and the like, and four compounds can be prepared through separation. Results of structure identification show that one of the four compounds is an anthocyanin compound, specifically delphinidin-3-O-elderberry bioside; the four compounds further comprise three flavone compounds, specifically rutin, quercetin-3-O-glucoside and quercetin-3-O-rhamnoside. The product prepared by using the method through separation is high in purity, the flavone compound is relatively good in bioactivity, and basesfor preparation of standard flavone products and further development and utilization of symplocos paniculata fruits are made according to research results.

Description

technical field [0001] The invention relates to the technical field of separation and purification of compounds, in particular to a preparation method for high-speed countercurrent chromatography of white sandalwood compound. Background technique [0002] White sandalwood (Symplocos Paniculata (Thunb) Miq.) is a small tree or deciduous shrub of the genus Paniculata (Symplocos Paniculata (Thunb) Miq.), also known as black seed and broken seed tree. It is widely distributed all over the world. Developed, it is an ideal plant for preventing soil erosion and improving the ecological environment in low mountain and hilly areas; at the same time, its fruits, roots, flowers, etc. have high economic value and medicinal value. Among them, the fruit of white sandalwood turns blue or blue-purple when ripe, and is edible and used as medicine. The oil content of the seeds in the fruit is 36.6%, and it contains two kinds of unsaturated fatty acids necessary for the human body, namely ole...

Claims

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Application Information

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IPC IPC(8): C07H17/065C07H17/07C07H1/08
CPCC07H1/08C07H17/065C07H17/07
Inventor 张良波陆英李昌珠李培旺彭晓英陈景震皮兵刘强
Owner 张良波
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