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Method for extracting, separating and purifying triglochin palustre acid

A technology for separation and purification of Ophiopogon acid, applied in the separation/purification of carboxylic acid compounds, material separation, analysis of materials, etc., can solve the problems of inability to characterize, difficult to identify, and not rigorous enough, and achieves a simple, fast and effective identification process. The method is stable and reliable, and the steps are simple.

Active Publication Date: 2017-06-13
CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to seek profit, there are many traders who processed tiger palms and then screened and polished them. The original sub-tubers have no obvious characteristics and are very similar to pinellia, making it difficult to identify them. If they are processed into decoction pieces, they can hardly be identified by their characteristics.
At present, there are still many problems in the identification of Pinellia and tiger palm. Traditionally, Pinellia is spherical or oval, and generally has no sub-tubers. However, there are cultivation variations in cultivated Pinellia, and some cultivated Pinellia medicinal materials have sub-tubers. Yes, this has caused the identification of Pinellia and Tiger's Palm by the presence or absence of sub-tubers, and there is a problem of inaccurate identification. Some judge Pinellia and Tiger's Palm by the number of sub-tubers (more than 3 are judged as Tiger's Palm) ), this method is still not rigorous enough
[0005] There is no report on the extraction and separation method of lysopogonic acid at present, only the literature reports that there is lysotropin in the flower of lysopogon japonicus, and lysotropin can be obtained by hydrolysis, but there is no standard product of lysotropic acid and Extraction, separation and purification method

Method used

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  • Method for extracting, separating and purifying triglochin palustre acid
  • Method for extracting, separating and purifying triglochin palustre acid
  • Method for extracting, separating and purifying triglochin palustre acid

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Experimental program
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Effect test

Embodiment 2

[0054] The identification method of embodiment 2 pinellia of the present invention, tiger's palm

[0055] 1. Preparation of reference solution

[0056] Take an appropriate amount of water as the reference substance of lysoporic acid, add mobile phase to dissolve, and make a solution with a concentration of 0.05 mg / ml.

[0057] 2. Preparation of the test solution

[0058] Take 1g of pinellia or tiger palm medicinal powder, add 20ml of water, ultrasonically extract for more than 30min, filter or centrifuge, take 10ml of clarified extract, add 0.1ml of phosphoric acid, extract with ethyl acetate 4 times, 20-30ml each time, recover ethyl acetate Esters, the residue was dissolved in 5ml mobile phase, passed through a microporous membrane, and obtained.

[0059] 3. Chromatographic conditions

[0060] Mobile phase: A (acetonitrile)-B (0.1% phosphoric acid) (3:97)

[0061] Column: Agilent ZORBAX Eclipse Plus C 18 Liquid chromatography column (4.6×250mm, 5μm)

[0062] Flow rate: ...

Embodiment 3

[0068] Embodiment 3 extraction method condition screening test of the present invention

[0069] 1. Investigation of extraction method

[0070] (1) The amount of extraction solvent

[0071] Weigh 1g of tiger palm sample, add 20ml, 30ml, 40ml of water respectively, ultrasonically extract, take 10ml of clarified extract respectively, add 0.1ml of acid, extract with ethyl acetate, recover the solvent, dissolve with 5ml of mobile phase solution, pass through a microporous membrane , detected by high performance liquid chromatography.

[0072] Table 3 Investigation of Extraction Solvent Consumption

[0073] water consumption 20ml 30ml 40ml Water lysoic acid peak area 162 102 70 Converted peak area 162 153 140

[0074] When the water volume is 20ml, the peak area is the highest and the extraction effect is the best.

[0075] (2) Investigation of extraction time

[0076] Weigh 1g of tiger palm sample, add 20ml of water, and extract by ultrasonic....

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Abstract

The invention discloses a method for extracting, separating and purifying triglochin palustre acid from pedate pinellia. The method is characterized by comprising the following steps: (a) fetching the medicinal materials, namely pedate pinellia, grinding, adding water and mixing uniformly, and performing ultrasonic extraction; (b) filtering the extract, adding phosphoric acid into the filtrate, and extracting with ethyl acetate; (c) fetching the ethyl acetate layer and pressurizing and concentrating to be dry; and adding water for dilution and filtering to obtain an aqueous solution; (d) treating the water liquid on a C18 preparation column, eluting a mobile phase with 3-5% of acetonitrile and 0.2% of phosphoric acid, monitoring at 210nm at a flowing speed of 140ml / min, and performing fractional collection of the eluent; (e) concentrating the eluent; and (f) further treating the concentrate with the C18 preparation column, eluting the mobile phase with 3-5% acetonitrile and 0.1% formic acid, monitoring at 210nm at a flowing speed of 140ml / min, and collecting the eluent; and performing freeze drying to obtain white solid which is the compound provided by the invention. According to the method for extracting, separating and purifying triglochin palustre acid from pedate pinellia disclosed by the invention, the steps are simple, and the prepared triglochin palustre acid has relatively high purity; the triglochin palustre acid is used for identifying whether pinellia ternata is adulterated by pedate pinellia; and if triglochin palustre acid is contained, the pinellia ternata is adulterated by pedate pinellia. The identifying process is simple, fast and effective and can be used for identifying pedate pinellia and identifying whether the pinellia ternata is adulterated by pedate pinellia; the pedate pinellia subjected to preparation still can be identified; and the method is stable and reliable.

Description

technical field [0001] The present invention relates to a compound and its separation and purification method. Background technique [0002] Pinellia is the dry tuber of Pinellia ternata (Thunb.) Breit, a plant of the genus Pinellia in the family Araceae. Tiger palm is the dried tuber of Pinelliae Pedatisecta Schott, a plant of the genus Pinellia in the family Pinellia. [0003] There are many counterfeit products of Pinellia, mainly Tiger Palm, Araceae, and Pinellia of the family Araceae. Planting medicinal materials, illegally seeking profits, seriously damaging the interests of pinellia growers and producing enterprises of pinellia decoction pieces, and also seriously affecting the quality, curative effect and drug safety of pinellia. [0004] At present, tiger's palm is a common adulterant in pinellia, and the identification method of pinellia and tiger's palm is mainly based on character identification, but the identification is very difficult. Pinellia and tiger pal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C57/02G01N30/06
CPCC07C51/42G01N30/06C07C57/02
Inventor 李敏敬勇陈辉陶玲何金晓刘佳灵
Owner CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE