Preparation method of pectolinarin reference substance

A technology for crude fish leaf glycosides and fish leaf glycosides, which is applied in the field of modernization of traditional Chinese medicine, and can solve problems such as poor solubility of fish leaf glycosides, difficulty in separating monomers, and insufficient supply

Active Publication Date: 2020-02-25
上海诗丹德标准技术服务有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are few domestic literature reports on the separation and purification of leaf glycosides from Salmonella lanceolata. In addition, leaf glycosides from Salmonfish lanceolata have been listed as standards in the 2015 edition of the Pharmacopoeia, and the demand for them is increasing. Very poor, it is very difficult to separate the monomer from medicinal materials, and the supply in the market is seriously insufficient. Therefore, it is very necessary to separate and purify the reference substance of the leaf glycosides from thistle, which has wide application value

Method used

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  • Preparation method of pectolinarin reference substance
  • Preparation method of pectolinarin reference substance

Examples

Experimental program
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Embodiment 1

[0059] The preparation method of the leaf glucoside reference substance of Liu Chuanyu is characterized in that it is carried out according to the following process steps:

[0060] A. Raw material extraction: add 180L ethanol solution with a volume fraction of 70% to 30Kg of thistle medicinal material, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, filter with suction, combine filtrates, concentrate to no alcohol Flavor, 10L in total;

[0061] B. Macroporous resin enrichment: Weigh 6KgAB-8 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 15 hours overnight, and then use 30% of 25L water and 20L column volume respectively Elute the impurities with ethanol solution, then elute the target substance with 10L of 60% ethanol solution, collect the eluent, and concentrate to 400ml;

[0062] C. Polyamide purification: add 3% NaOH solution to the concentrated s...

Embodiment 2

[0069] A. Raw material extraction: Add 100Kg of thistle medicinal material, add 600L ethanol solution with a volume fraction of 70%, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, filter with suction, combine the filtrates, and concentrate to no alcohol Flavor, 30L in total;

[0070] B. Macroporous resin enrichment: Weigh 20KgAB-8 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 15 hours overnight, and then use 30% of 80L water and 50L column volume respectively Elute the impurities with ethanol solution, then elute the target substance with 30L of 60% ethanol solution, collect the eluent, and concentrate to 1000ml;

[0071] C. Polyamide purification: add 3% NaOH solution to the concentrated solution of step B to dissolve, mix the sample with polyamide 1:1, add 3% hydrochloric acid to adjust to neutrality, dry, perform polyamide column chromatography, ...

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Abstract

The invention discloses a preparation method of a pectolinarin reference substance. In particular, the method of the present invention comprises the steps of: (i) providing an alcohol extract of pectolinarin; (ii) dissolving the alcohol extract by using a NaOH aqueous solution, separating the alcohol extract by using a polyamide column through an eluent, and performing concentrating to obtain a semi-finished product of the pectolinarin; (iii) dissolving the semi-finished product of the pectolinarin, and separating the semi-finished product by utilizing a medium-pressure preparation column so as to obtain a crude product of the pectolinarin; (iv) carrying out alkali dissolution and acid precipitation on the crude product of the pectolinarin, filtering to obtain a solid, carrying out hot dissolution and cold precipitation on the solid by using methanol, and carrying out suction filtration to obtain a pure product of the pectolinarin; and (v) concentrating and freeze-drying the pure product to obtain the pectolinarin reference substance. The method is stable in process, convenient to operate, high in separation efficiency, low in cost, economical and environmentally friendly, and hashigh economic value and academic value.

Description

technical field [0001] The invention belongs to the technical field of modernization of traditional Chinese medicine, and relates to a preparation method of a chemical reference substance of traditional Chinese medicine. Specifically, the invention provides a preparation method of a reference substance of salicyloside leaf glycoside. Background technique [0002] Large thistle is the dry aboveground part of Cirsium japonicum Fisch.ex DC., which is a plant in the Compositae family. The aboveground part is harvested when the flowers bloom in summer and autumn, removed from impurities, and dried in the sun. The chemical components of thistle mainly include triterpenes and steroids, volatile oils, flavonoids and flavonoid glycosides, long-chain enynols, organic acids and other compounds. Clinically, thistle is sweet in taste, slightly bitter, cool in nature, and has the functions of "eliminating congestion, generating new blood, stopping vomiting blood, stopping nosebleeds and e...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/06
CPCC07H17/07C07H1/06Y02A50/30
Inventor 舒亚平杨士杰贺湘钱勇谢天培
Owner 上海诗丹德标准技术服务有限公司
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