Preparation method for high-purity glabridin monomer
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A high-purity technology of glabridin, which is applied in organic chemistry and other fields, can solve the problems of low-purity glabridin, low content, and long separation time, and achieve the effects of rapid preparation, separation, mild separation environment, and short separation time
Active Publication Date: 2016-02-03
HUBEI ARTEC CARBOHYDRATE CHEM
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[0002] Known licorice is a leguminous plant licorice ( Glycyrrhizauralensis Fisch.), Glycyrrhiza inflate ( Glycyrrhizainflate Bat.), or Glycyrrhiza glabra ( Glycyrrhiza glabra L) dry roots and rhizomes; licorice is sweet in taste, flat in nature, and non-toxic. It is a tonic traditional Chinese medicine, which has the functions of nourishing qi and invigorating the middle, relieving spasms and relieving pain, moistening the lungs and relieving cough, purging fire and detoxification, and reconciling various medicines; licorice glabra Glabridin is a unique isoflavone component of Glycyrrhizae glabra. Studies have shown that glabridin has strong antioxidant activity, in addition to anti-atherosclerosis, lowering blood lipids, neuroprotection, enhancing memory, inhibiting melanin formation, Weight loss and other effects; Glabridin is the most expensive natural freckle-removing and whitening raw material in the world. Traditional methods such as extraction, silica gel column chromatography, recrystallization and liquid preparation are used to separate and purify glabridin monomer. The above-mentioned separation and purification process is complicated, the separation efficiency is low, the separation time is long, and the solvent consumption is large. Therefore, high-purity glabridin very expensive
Patent application numbers 200410079233.1 and 200880117804.2 are low-purity licorice glabridin products with a purity of only about 50%. Certain purity also can only reach more than 90%, can not satisfy the requirement of standard substance and reference substance; Patent application number is 200910311302.X adopts efficient preparation liquid phase method and can obtain the glabridin with purity greater than 98%, but solvent consumption is too much large, long separation time
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Embodiment 1
[0022] Take 3kg of licorice, crush it, and put it at 40~80 0 Under the temperature of C, within 1~2 hours, reflux extraction with 70% ethanol for 3 times, each time for 1h, the extracts were combined and then concentrated under reduced pressure to obtain 162g of extract, which was enriched with licorice root by reverse phase C18 column chromatography 4L of 30%, 50%, 70% and 95% ethanol / water were used for elution, and the 70% ethanol eluate was collected, detected by HPLC, and concentrated to dryness under reduced pressure to obtain 28g of crude glabridin.
[0023] Preparation of high-purity glabridin monomer:
[0024] Using a preparative high-speed countercurrent chromatograph, the separation solvent is selected from petroleum ether, ethyl acetate, ethanol and water to separate and prepare high-purity glabridin monomer from the crude product of glabridin; first, the above-mentioned Configure 2L of separation solvent in a separatory funnel, shake well, let stand for 12 hours,...
Embodiment 2
[0027] Take 3kg of licorice, crush it, and put it at 40~80 0 Under the temperature of C, within 1 to 2 hours, reflux extraction with 90% ethanol for 3 times (1 hour each time), the extracts were combined and concentrated under reduced pressure to obtain 171g of extract; the extract was enriched with glabridin by reverse phase C18 column chromatography , sequentially eluted with 4 L of 30%, 50%, 70% and 95% ethanol / water, collected 70% ethanol eluate, detected by HPLC, concentrated under reduced pressure to dryness to obtain 28 g of crude glabridin.
[0028] Preparation of high-purity glabridin monomer:
[0029]High-purity glabridin monomer was separated from crude glabridin by using a preparative high-speed countercurrent chromatograph, and the separation solvent was n-hexane, ethyl acetate, ethanol and water. First, configure 2L of the above solvent system in a separatory funnel with a volume ratio of 5:5:5.5:4.5, shake it up and let it stand for 12 hours to separate layers....
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Abstract
The invention relates to a preparation method for a high-purity glabridin monomer, and relates to the preparation method for the high-purity glabridin monomer by separation from licorice. The preparation method mainly solves the problems of complicated preparation process, low separation efficiency, long separation time, and large consumption amount of a solvent. The method provided by the invention is characterized by comprising the following steps: preparation of a glabridin extract; concentration of glabridin by using a reversed-phase C18 column chromatography: successively eluting the extract with alcohols respectively with a concentration of 50%, 70% and 95%, respectively collecting eluents, and subjecting the collected eluent of the alcohol with the concentration of 70% to vacuum concentration until the eluent is dried so as to obtain crude glabridin; and separation of the above-mentioned crude glabridin with a high-speed countercurrent chromatographic technology: placing a separating solvent in a separatory funnel and carrying out complete shaking, then carrying out standing and layering, dissolving the above-mentioned crude glabridin in the separating solvent, and respectively measuring the concentrations of supernatant and subnatant solutions containing the glabridin with a highly-efficient liquid-phase chromatographic method. The preparation method for the high-purity glabridin monomer provided by the invention has short separation time and high recovery rate, is free of pollution, and saves the solvent.
Description
technical field [0001] The invention belongs to the technical field of separation and purification of active components of traditional Chinese medicines, and in particular relates to a preparation method for separating and preparing high-purity glabridin monomer from licorice. Background technique [0002] Known licorice is a leguminous plant licorice ( Glycyrrhizauralensis Fisch.), Glycyrrhiza inflate ( Glycyrrhizainflate Bat.), or Glycyrrhiza glabra ( Glycyrrhiza glabra L) dry roots and rhizomes; licorice is sweet in taste, flat in nature, and non-toxic. It is a tonic traditional Chinese medicine, which has the functions of nourishing qi and invigorating the middle, relieving spasms and relieving pain, moistening the lungs and relieving cough, purging fire and detoxification, and reconciling various medicines; licorice glabra Glabridin is a unique isoflavone component of Glycyrrhizae glabra. Studies have shown that glabridin has strong antioxidant activity, in addition...
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