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Method for separating and purifying linarin monomers

A technology for separation and purification of fenugreek, which is applied in chemical instruments and methods, chemical recovery, organic chemistry, etc., can solve the problem of inability to obtain high-purity fenugreek monomer, and achieve easy expansion of production and stable process Reliable, high-yield results

Active Publication Date: 2015-07-08
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims to solve the technical problem that mongoside monomer cannot obtain high-purity mongoside from crystallization, and provides a separation and purification method of mongoside monomer

Method used

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  • Method for separating and purifying linarin monomers
  • Method for separating and purifying linarin monomers
  • Method for separating and purifying linarin monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] A method for separation and purification of mongolin monomer, including the following process steps:

[0048] (1) Extraction

[0049] Take 1kg of wild chrysanthemum medicinal material, crush it into coarse powder with a diameter of 3mm, add 10L of 95% ethanol solution, reflux and extract 3 times, 2 hours each time, filter, collect and combine the filtrate;

[0050] (2), concentration

[0051] Recover ethanol from the filtrate collected and combined in step (1). When it is concentrated to 3L, let stand for 12 hours at room temperature to crystallize, filter and collect the precipitate, remove the filtrate (the filtrate mainly contains some pigments and large polar impurities), and remove the precipitate After drying at 60°C (weight 18 grams), proceed to the next solvent washing treatment;

[0052] (3) Solvent washing

[0053] Add 180 mL of methanol to the precipitate obtained in step (2) for ultrasonic washing. After the product and methanol become a suspension, filter with medium...

Embodiment 2

[0069] A method for separation and purification of mongolin monomer, including the following process steps:

[0070] (1) Extract

[0071] Take 10kg of wild chrysanthemum medicinal material, crush it into coarse powder with a diameter of about 3mm, add 100L of 95% ethanol solution, reflux and extract 4 times, 2 hours each time, filter, collect and combine the filtrate;

[0072] (2) Concentration

[0073] Recover ethanol from the filtrate collected and combined in step (1), concentrate to about 35L, stand for 10 hours at room temperature to crystallize, filter to collect the precipitate, and remove the filtrate (the filtrate mainly contains some pigments and large polar impurities). After the precipitation is dried (weight 192 grams), proceed to the next solvent washing treatment;

[0074] (3) Solvent washing

[0075] Add 1.92L of methanol to the precipitate obtained in step (2) for ultrasonic washing, and after sufficient washing, filter with medium-speed filter paper to collect and filt...

Embodiment 3

[0091] A method for separation and purification of mongolin monomer, including the following process steps:

[0092] (1) Extract

[0093] Take 50kg of wild chrysanthemum medicinal materials, crush them into coarse powder with a diameter of about 3mm, add 500L of 95% ethanol solution, reflux and extract 3 times, 2 hours each time, filter, collect and combine the filtrate;

[0094] (2) Concentration

[0095] Recover ethanol from the filtrate collected and combined in step (1), concentrate to about 150L, ​​let stand for 11 hours at room temperature to crystallize, filter and collect the precipitate, and remove the filtrate (the filtrate mainly contains some pigments and large polar impurities), and After the precipitation is dried (weight 1012g), proceed to the next solvent washing treatment;

[0096] (3) Solvent washing

[0097] Add 10.12L of methanol to the precipitate obtained in step (2) for ultrasonic washing. After the product and methanol become a suspension, filter with a medium-sp...

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Abstract

The invention provides a method for separating and purifying linarin monomers. The method comprises the following processing steps: (1), extraction: a wild chrysanthemum flower medicinal material is subjected to reflux extraction by an ethanol solution, and a filtrate is collected; (2), concentration: after the concentration, the filtrate is subjected to still standing, crystallization, drying and precipitating; (3), solvent washing: the precipitation is subjected to ultrasonic washing by methyl alcohol and filtered, and solids are collected, filtered and dried; (4), dissolution and filtration: an organic solvent is added into the dried solids, the solids are filtered, and filtrate is collected; (5), efficient preparative liquid phase chromatograph separation: preparation fraction solutions of linarin monomers are purposefully collected, and a solution of linarin monomers is obtained; and (6), product recycle: acetonitrile is recycled, and after the linarin monomers are dissolved out, the linarin monomer product is obtained by drying. The method for separating and purifying the linarin monomers has the advantages that the operation is simple and convenient, the production cycle is short, the separation efficiency is high, the processing is stable, and the cost is easy to control, so that high purity separating preparation of a large quantity of linarin monomers can be realized; and moreover, the purity of the linarin monomers is high, so that the linarin monomers can be used as comparison substances for the content determination.

Description

technical field [0001] The invention relates to a method for isolating compound monomers from plants, in particular to a method for separating and purifying mongoside monomers from wild chrysanthemums, and belongs to the technical field of separation and purification of compound monomers. Background technique [0002] Wild chrysanthemum (Flower of Indian Dendranthema, Wild chrysanthemum) is the flower head of wild chrysanthemum, a perennial herb of Compositae, which is similar in appearance to chrysanthemum. The product is yellow, sessile, complete, fragrant, and the flowers are not fully bloomed. Wild chrysanthemum can be widely used in the treatment of furuncle carbuncle, sore throat, wind-fire red eyes, headache and dizziness and other diseases. At the same time, it has a good antihypertensive effect and can be used as an adjuvant treatment for hypertension. [0003] Buddleoside is a characteristic chemical component of wild chrysanthemum, and it is also the most active...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCY02P20/582
Inventor 白兰辉文焕松夏柯郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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