CN1359905A

CN1359905A - Process for extracting licoflavone, lycyrrhizic acid and licopolyose from liquorice root

Info

Publication number: CN1359905A
Application number: CN 01130599
Authority: CN
Inventors: 刘钢; 匡军
Original assignee: Ningxia University
Current assignee: Ningxia University
Priority date: 2001-12-15
Filing date: 2001-12-15
Publication date: 2002-07-24

Abstract

A process for extracting licoflavone, glycyrrhizic acid and licopolyose from licorice root incldues such steps as extracting licoflavone using alcohol, extracting glycyrrhizic acid from residual dregs using alkaline clean water, boiling its residual dregs in clean water, and alcohol separating to prepare licopolyose. Its advantages are continuous extraction and the highest utilization rate.

Description

System separates, extracts licoflavone, Potenlini, licorice polysaccharide production method from Radix Glycyrrhizae

Technical field

The invention belongs to medicine, chemical field, particularly a kind of method of from Radix Glycyrrhizae, extracting licoflavone, Potenlini and licorice polysaccharide continuously.

Background technology

Licoflavone, Potenlini, licorice polysaccharide is a main pharmaceutically-active ingredients in the Radix Glycyrrhizae, existing extractive technique is intermittent, often extract Potenlini or the residue after extract merely by a cover system, extract licoflavone or licorice polysaccharide in the waste liquid, Chinese patent " a kind of licorice root ointment and production technique thereof " (CN1144105) disclose a kind of from Radix Glycyrrhizae, extract glycyrrhizin after, residue extracts the method for licoflavone again, comprise that the prior art of above-mentioned technology does not all fully take into account the chemical structure of each composition in the Radix Glycyrrhizae, adopted irrational division and extracting method, cause some effective by force, the composition of low levels is cut apart by unreasonable, destroyed and run off, thus make the precious wild Radix Glycyrrhizae resource that lacks day by day fail to be utilized fully.

Summary of the invention

The purpose of this invention is to provide a kind of easy, reasonable, can continuously licoflavone, Potenlini, licorice polysaccharide be effectively separated and yield and the higher method of each composition purity.

Purpose of the present invention realizes by following scheme:

System separates, extracts licoflavone, Potenlini, licorice polysaccharide production method from Radix Glycyrrhizae, its technological process divided for three steps, the first step extraction using alcohol licoflavone, second step was extracted Potenlini with the first step residue with alkaline clear water, and the 3rd step was residue obtainedly produced licorice polysaccharide with separating out alcohol method after boiling extraction with clear water with second step;

Above-mentioned the first step technological process be with licorice powder and high concentration ethanol by weight 1: 5-8 is blended in 60-70 ℃ of heating and extracted 3-5 hour, cool off again, filter, wash, repeat again to extract once, merge extracted twice liquid and washing lotion, add elutriation after concentrating and go out precipitation, more after filtration, vacuum-drying gets the Radix Glycyrrhizae crude flavonoid powder;

The above-mentioned second step process process is the first step to be extracted the back residue slough to add behind the ethanol and soak 9-12 hour after-filtration, washing in the weakly alkaline clear water, repeat again to extract twice, merge three filtrate and washing lotion, adding acid, to be neutralized to pH value be that 2-3 separates out precipitation, leave standstill the back suction and remove supernatant liquor, washing of precipitate is filtered the back airing or is dried to such an extent that Radix Glycyrrhizae is slightly sour;

Above-mentioned three step process process is that the residue after second step was extracted adds its weight 7-9 times water boil 6-8 hour, cooling, filter, washing, repeat again once, merge twice filtrate and washing lotion, add dense ethanol behind the concentrating under reduced pressure and separate out precipitation, get thick licorice polysaccharide after filtration, the vacuum-drying.

The present invention is in abundant research, analyze the structure of each effective ingredient in the Radix Glycyrrhizae, on the basis of character and the existence form in Radix Glycyrrhizae thereof, adopted a rational system, continuous isolating method, can be to greatest extent with licoflavone, Potenlini, licorice polysaccharide is separated from Radix Glycyrrhizae, prevent some effective ingredient in the Radix Glycyrrhizae, particularly effectively strong, the low levels composition is cut apart because of unreasonable separation, destroyed and run off, the yield of licoflavone is enhanced about more than once, Potenlini, the purity of licorice polysaccharide also increases, for further refining, purifying has been created good condition.

Embodiment

100 gram licorice powders are added in the 1000ml there-necked flasks, add the ethanol 600ml of 90% (weight), 60 ° of-70 ℃ of heated and stirred 5 hours, vacuum filtration, washing, residue repeats to extract once again, merging filtrate and washing lotion, heating is concentrated into 50ml, reclaims ethanol, add 500ml water in the concentrated solution, separate out precipitation, refilter, filter cake gets crude flavonoid powder 12 grams 80 ℃ of following vacuum-dryings, content 40.06% (weight) gets residue I, is used for next procedure.

I flings to ethanol with residue, put into the 1500ml beaker, add 0.5% (weight) weak ammonia 1000ml, intermittently stir and soaked 10 hours, filtration, washing, filter residue repeat to extract secondary again, merging filtrate and washing lotion, adding sulfuric acid, to be neutralized to pH value be 2, separates out precipitation, leaves standstill the back and inhale and remove supernatant liquor, precipitation uses vacuum filtration, washing leaching cake to dry to such an extent that the thick acid 10 of khaki color Radix Glycyrrhizae restrains.Get residual II, be used for next procedure.

Residual II is dropped in the 1000ml there-necked flask, add 800ml water, boiled 8 hours, filter, wash, repeat once merging filtrate and washing lotion again, be evaporated to 50ml, the alcohol that adds 95% (weight) of 8 times of amounts, sedimentation and filtration, washing, 80 ℃ of vacuum-dryings, get Crude polysaccharides 5 grams, contain polysaccharide 27.52% (weight), be the field gray powder.

Claims

1. system separates, extracts licoflavone, Potenlini, licorice polysaccharide production method from Radix Glycyrrhizae, it is characterized in that its technological process divided for three steps, the first step extraction using alcohol licoflavone, second step was extracted Potenlini with the first step residue with alkaline clear water, and the 3rd step was residue obtainedly produced licorice polysaccharide with separating out alcohol method after boiling extraction with clear water with second step.

2. the production method of system's separation from Radix Glycyrrhizae as claimed in claim 1, extraction licoflavone, Potenlini, licorice polysaccharide, it is characterized in that above-mentioned the first step technological process is with licorice powder and high concentration ethanol by weight 1: 5-8 mixes, extracted 3-5 hour 60-70 ℃ of heating, cool off again, filter, wash, repeat again to extract once, merge extracted twice liquid and washing lotion, add elutriation after concentrating and go out precipitation, more after filtration, vacuum-drying gets the Radix Glycyrrhizae crude flavonoid powder.

3. the production method of system's separation from Radix Glycyrrhizae as claimed in claim 1, extraction licoflavone, Potenlini, licorice polysaccharide, it is characterized in that the above-mentioned second step process process is that residue after the first step is extracted is sloughed to add behind the ethanol and soaked 9-12 hour after-filtration, washing in the weakly alkaline clear water, repeat again to extract twice, merge three filtrate and washing lotion, adding acid, to be neutralized to pH value be that 2-3 separates out precipitation, leave standstill the back and inhale and to remove supernatant liquor, behind the sedimentation and filtration airing or dry slightly acid of Radix Glycyrrhizae.

4. the production method of system's separation from Radix Glycyrrhizae as claimed in claim 1, extraction licoflavone, Potenlini, licorice polysaccharide, it is characterized in that above-mentioned three step process process is that residue after second step was extracted adds doubly water boil 6-8 hour of its weight 7-9, cooling, filtration, washing, repeat again once, merge twice filtrate and washing lotion, add dense ethanol behind the concentrating under reduced pressure and separate out precipitation, get thick licorice polysaccharide after filtration, the vacuum-drying.