CN1318440C - Preparation method of low-acid ginkgo leaf extract - Google Patents
Preparation method of low-acid ginkgo leaf extract Download PDFInfo
- Publication number
- CN1318440C CN1318440C CNB031148263A CN03114826A CN1318440C CN 1318440 C CN1318440 C CN 1318440C CN B031148263 A CNB031148263 A CN B031148263A CN 03114826 A CN03114826 A CN 03114826A CN 1318440 C CN1318440 C CN 1318440C
- Authority
- CN
- China
- Prior art keywords
- acetone
- resin
- elutriant
- preparation
- folium ginkgo
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a method for preparing low-acidity gingko leaf extract, which comprises that ginkgo leaves are used as a material to be extracted by aqueous ethanol or methanol or acetone, a solvent is concentrated and recovered by an extracting solution, and a concentrated solution is diluted by water or purifying water to be cooled and sedimentated at below 20 DEG C; supernatant fluid is sprayed on a macroporous adsorptive resin column to be adsorbed and eluted by an alcohol solution, eluent is adsorbed by a deacidifying resin column and is eluted by the alcohol solution, and effluent liquid and the eluent are merged to be concentrated and dried at below 75 DEG C or the gingko leaf extract is used as a material to be dissolved by the alcohol solution and an acetone solution, a dissolved solution passes the deacidifying resin column to be adsorbed and is eluted by the alcohol solution and the acetone solution, effluent liquid and eluent are merged to be concentrated and dried at below 75 DEG C. the preparation method has the advantages of simple process flows, short periods, favourable effect of removing ginkgol acid, no harmful residues of used media, good product quality, stable technology and low cost.
Description
The invention belongs to the extractive technique of the medicinal composition of natural phant, specifically a kind of preparation method of extractive of low acidic gingko leaves.
Ginkgo Ginkgoaceae ginkgo kind of plant, be one of the most ancient seeds, its fruit and leaf are Chinese medicinal materials commonly used, has the gas of astringing the lung, relieving asthma and cough, only with turbid function, can be used for treating the deficiency syndrome of the lung coughs and breathes heavily, coronary heart disease, diseases such as stenocardia, the Folium Ginkgo extract that extracts from Ginkgo Leaf is made various preparations, arteriosclerosis and caused by hypertension coronary insufficiency have been widely used in, stenocardia, myocardial infarction, cerebral thrombosis, diseases such as cerebral vasospasm, in recent years, medical science man both domestic and external has done a large amount of effort to Ginkgo Leaf exploitation, discovery is in Folium Ginkgo extract, the effective active that accounts for main ratio is male along being flavones, flavonol and examination class thereof, catechin element and bisflavones, the interior lipid of sesquiterpene and diterpene, but also found wherein to contain consequently strong allergy of human body and the phenolic acids mixture that causes illness such as contact dermatitis, be referred to as ginkgolic acid, experimental results show that, ginkgolic acid content in this Folium Ginkgo extract must be just harmless in 10ppm, and world's first ginkgo symposial in 1997 has proposed the oxious component ginkgolic acid content in the Folium Ginkgo extract product is reduced to standard below the 5ppm.But also do not reach this requirement in the domestic most Semen Ginkgo extrac at present.
The object of the present invention is to provide the preparation method of the almost nil extractive of low acidic gingko leaves of a kind of stable and suitable industrialized production, ginkgolic acid content.
Realize the technical scheme of the object of the invention: it mainly comprises the following steps:
With the Ginkgo Leaf is raw material:
(a) Ginkgo Leaf 40%-95% ethanol or 40%-100% methyl alcohol or 40%-100% acetone extraction;
(b) get extracting solution and concentrate recovery ethanol or methyl alcohol or acetone;
(c) concentrated solution dilution cooling is one 1 ℃ to 20 ℃ sedimentations;
(d) supernatant liquor is crossed the absorption of styrene tyle macroporous adsorption resin post;
(e) with alcohols or acetone soln wash-out;
(f) elutriant is crossed DAD-1 deacidification resin column absorption liposoluble ingredient;
(g) with alcohols or acetone soln wash-out;
(h) effluent liquid and elutriant concentrate drying;
Step in aforesaid method (e) can be a wash-out, and eluent is good with ethanol or methyl alcohol or acetone, concentration 30%-95%.
Step in aforesaid method (e) can be a gradient elution, and eluent is good with ethanol or methyl alcohol or acetone, and wash-out concentration is 0%-30% for the first time; Wash-out concentration is 40%-95% for the second time;
The eluent of step in aforesaid method (g) is methyl alcohol or ethanol or acetone, and its concentration can be 30%-95%;
The thinner that the concentrated solution dilution is adopted in step (c) in aforesaid method can be water or purified water;
Step in aforesaid method (c) also can be concentrated solution dilution back roughing out, redilution, cooling natural subsidence;
Can be in the step in aforesaid method (a) that dipping extracts, temperature range is a normal temperature to 80 ℃;
Step in aforesaid method (h) elutriant thickening temperature is less than 75 ℃.
The preparation method of a kind of extractive of low acidic gingko leaves of the present invention, technical process is simple, and the cycle is short, and it is effective to remove ginkgolic acid, and the medium unharmful substance that is adopted is residual, superior product quality, cost is low.
The present invention is further illustrated below in conjunction with embodiment, but the present invention also is not limited only to the content of embodiment.
Embodiment one:
Get Ginkgo Leaf 1kg, with 40% ethanol 12,10,10 times (refer in raw material weight and solvent volume ratio, subsequent embodiment and uppermost leaf order are together), 80 ℃ are stirred dipping and extract three times, each 2 hours, emit extracting solution, merge and to be concentrated into small volume, add the purified water dilution of 5 times of amounts, under 0 ℃ or-1 ℃ of temperature, left standstill 12 hours through the purified water that the soup after the roughing out the adds 5 times of amounts again back that stirs, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) AB-8, with the washing of 2 times of resin volumes, behind 20% ethanol elution, resin is used 75% ethanol elution again, collect elutriant, elutriant is directly crossed DAD-1 and is removed acid resin, with 75% an amount of ethanol elution, collects and merging effluent liquid and elutriant, concentrating under reduced pressure, drying under reduced pressure then, controlled temperature≤75 ℃, the apricot yellow keto-alcohol glycosides 28.5% of argentiferous, Folium Ginkgo terpene lactones is 7.5%, and ginkgolic acid is the extractive of low acidic gingko leaves 25g of 2.38ppm.AB-8 resin ester and DAD-1 resin are reused after diverse ways is handled.
Embodiment two:
Get Ginkgo Leaf 200kg, with 75% ethanol 10,6,5 times, 70 ℃ of stirring and leaching three times, each 3 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 8 times of amounts, add purified water after the soup roughing out and be settled to 800L, under 20 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) DM-130, with the purifying washing of 2 times of resin volumes, ethanol elution with 75%, collect elutriant, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 75% an amount of ethanol elution, collect and merging effluent liquid and elutriant, concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24% then, Folium Ginkgo terpene lactones 〉=6%, ginkgolic acid are the Folium Ginkgo extract 5.5kg of 3.45ppm.Resin is reusable after regenerating respectively.
Embodiment three:
Get Ginkgo Leaf 200kg and be ground into area≤1cm
2Fragment, with 40% acetone 17,14,13 times, 60 ℃ of lixiviates three times each 4 hours, are emitted vat liquor, merge and be concentrated into small volume, add the purified water dilution of 8 times of amounts, under 20 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-600, purifying washing with 2 times of resin volumes, acetone wash-out with 75%, elutriant are crossed the DAD-1 that has handled and are removed acid resin, with 75% an amount of acetone wash-out, collect and merging effluent liquid and elutriant, concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24% then, Folium Ginkgo terpene lactones 〉=6%, ginkgolic acid are the Folium Ginkgo extract 5.6kg of 1.23ppm.Resin is reused after diverse ways is handled.
Embodiment four:
Get Ginkgo Leaf 500kg and be ground into meal, with 40% methyl alcohol 10,6,5 times, 70 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the tap water dilution of 8 times of amounts, under 7 ℃, left standstill 4 hours, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-600 through the soup after the roughing out, purifying washing with 2 times of resin volumes, ethanol elution with 75% is collected elutriant, and elutriant is crossed the DAD-1 that has handled and removed acid resin, with 75% an amount of ethanol elution, collect and merging effluent liquid and elutriant ,≤75 ℃ of concentrating under reduced pressure, spraying dryings then, must contain flavonol glycosides 〉=24%, the ginkgolic acid of Folium Ginkgo terpene lactones 〉=6% is the Folium Ginkgo extract 14.5kg of 0.35ppm.Resin is reused after regenerating respectively.
Embodiment five:
Get Ginkgo Leaf 500kg, with 8,6,5 times of 85% ethanol, 55 ℃ of stirring and leaching three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the purified water dilution of 12 times of amounts, under 7 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) D101, purifying washing with 2 times of resin volumes, ethanol elution with 75%, elutriant are crossed the DAD-1 that has handled and are removed acid resin, with 75% an amount of ethanol elution, collect and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24% then, Folium Ginkgo terpene lactones 〉=6%, ginkgolic acid are the Folium Ginkgo extract 13.5kg of 0.13ppm.Resin is reused after regenerating respectively.
Embodiment six:
Get Ginkgo Leaf 1000kg and be ground into meal, with 95% ethanol 5,3,2 times, 60 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the purified water dilution of 10 times of amounts, under 10 ℃, left standstill 10 hours, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) AB-8 through the soup after the roughing out, purifying washing with 2 times of resin volumes, ethanol elution with 75%, elutriant are crossed the DAD-1 that has handled and are removed acid resin, with 75% an amount of ethanol elution, collect and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then, Folium Ginkgo terpene lactones 〉=10%, ginkgolic acid are the Folium Ginkgo extract 28kg of 1.23ppm.
Embodiment seven:
Get Ginkgo Leaf 1000kg and be ground into meal, with 8,6,5 times of 80% methyl alcohol, stirring at normal temperature lixiviate three times, each 5 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 10 times of amounts, under 10 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) ADS-17, with the purifying washing of 2 times of resin volumes, methanol-eluted fractions with 40%, elutriant is crossed the DAD-1 that has handled and is removed acid resin, collects elutriant.With 40% an amount of methanol-eluted fractions, collect and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then, the Folium Ginkgo extract 22kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment eight:
Get Ginkgo Leaf 1000kg and be ground into meal, with 95% methyl alcohol 8,6,6 times, 55 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merging is concentrated into small volume, adds the tap water dilution of 5 times of amounts, after roughing out, after the tap water that adds 5 times of amounts again stirs evenly, under 10 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-600, with the purifying washing of 2 times of resin volumes, ethanol elution with 95%, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 95% an amount of ethanol elution, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then, the Folium Ginkgo extract 28kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment nine:
Get Ginkgo Leaf 1000kg and be ground into meal, with 75% acetone 7,6,5 times, 80 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 1 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) D-101A, with the purifying washing of 2 times of resin volumes, acetone Shen with 95% is taken off, elutriant is crossed the DAD-1 that handled and is removed acid resin, and the acetone wash-out with an amount of 95% is collected also merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then, the Folium Ginkgo extract 25.8kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment ten:
Get Ginkgo Leaf 1000kg and be ground into meal, with 80% acetone 10,8,6 times, normal temperature lixiviate three times, each 6 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 10 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) ADS-16, with the purifying washing of 2 times of resin volumes, acetone wash-out with 40%, elutriant is crossed the DAD-1 that handled and is removed acid resin, and the acetone wash-out with an amount of 40% is collected also merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 25kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 11:
Get Ginkgo Leaf 1000kg and be ground into meal, with 92% acetone 10,8,6 times, stirring at normal temperature lixiviate three times, each 6 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 6 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) XDA-5, with the purifying washing of 2 times of resin volumes, ethanol elution with 75%, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 75% an amount of ethanol elution, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 25.8kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 12:
Get Ginkgo Leaf 1000kg and be ground into meal, with 100% acetone 10,8,6 times, 60 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 5 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-600, with the purifying washing of 2 times of resin volumes, methanol-eluted fractions with 70%, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 70% an amount of methanol-eluted fractions, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 26kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 13:
Get Ginkgo Leaf 1000kg and be ground into meal, with 95% methyl alcohol 10,8,6 times, stirring at normal temperature lixiviate three times each 6 hours, is emitted vat liquor, merge and be concentrated into small volume, add the purified water dilution of 10 times of amounts, after roughing out, under 10 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) LSA-20, with the purifying washing of 2 times of resin volumes, the acetone wash-out with 40%, elutriant are crossed the DAD-1 that has handled and are removed acid resin, acetone wash-out with an amount of 40%, collect and merging effluent liquid and elutriant, in≤75 ℃ of concentrating under reduced pressure, spraying drying, must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 23.5kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 14:
Get Ginkgo Leaf 1000kg and be ground into meal, with 95% industrial alcohol 8,8,7 times, 50 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 4 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) AB-8, with the purifying washing of 2 times of resin volumes, methanol-eluted fractions with 95%, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 95% an amount of methanol-eluted fractions, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, ≤ 75 ℃ of concentrating under reduced pressure dryings must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 25.8kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 15:
Get Ginkgo Leaf 1000kg and be ground into meal, with 90% industrial alcohol 12,12,10 times, 80 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 5 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) DM-130, with the purifying washing of 2 times of resin volumes, ethanol Shen with 75% is taken off, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 75% an amount of ethanol elution, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 24.5kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 16:
Get Ginkgo Leaf 1000kg and be ground into meal, with 95% medicinal alcohol 8,6,4 times, 70 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 3 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) ADS-17, with the purifying washing of 2 times of resin volumes, ethanol Shen with 70% is taken off, Shen is taken off liquid and is crossed the DAD-1 that handled and remove acid resin, with 70% an amount of ethanol elution, collects also merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 30.2kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 17:
Get Ginkgo Leaf 1000kg and be ground into meal, with edible ethanol 6,5,4 times, 65 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 10 ℃, leave standstill, get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) D140, with the purifying washing of 2 times of resin volumes, ethanol elution with 80%, elutriant is crossed the DAD-1 that has handled and is removed acid resin, with 80% an amount of ethanol elution, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 27.9kg of Folium Ginkgo terpene lactones 〉=8%.Resin is reused after diverse ways is handled.
Embodiment 18:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=9% Folium Ginkgo extract 30kg, after ethanol with 30% dissolves fully, solution is crossed the DAD-1 that has handled and is removed acid resin, with 30% an amount of ethanol elution, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 27.9kg of Folium Ginkgo terpene lactones 〉=8%.Resin is reused after diverse ways is handled.
Embodiment 19:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=9% Folium Ginkgo extract 30kg, after ethanol with 70% dissolves fully, solution is crossed the DAD-1 that has handled and is removed acid resin, with 70% an amount of ethanol elution, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 28.9kg of Folium Ginkgo terpene lactones 〉=8.5%.Resin is reused after diverse ways is handled.
Embodiment 20:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=6% Folium Ginkgo extract 30kg, after ethanol with 95% dissolves fully, solution is crossed the DAD-1 that handled and is removed acid resin with 95% an amount of ethanol elution, collect and merging effluent liquid and elutriant, in≤75 ℃ of concentrating under reduced pressure, spraying drying, must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 28kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 21:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=6% Folium Ginkgo extract 30kg, after methyl alcohol with 30% dissolves fully, solution is crossed the DAD-1 that has handled and is removed acid resin, with 30% an amount of methanol-eluted fractions, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 27.9kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 22:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=8% Folium Ginkgo extract 30kg, after methyl alcohol with 70% dissolves fully, solution is crossed the DAD-1 that has handled and is removed acid resin, with 75% an amount of methanol-eluted fractions, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 28.9kg of Folium Ginkgo terpene lactones 〉=8%.Resin is reused after diverse ways is handled.
Embodiment 23:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=6% Folium Ginkgo extract 30kg, after methyl alcohol with 95% dissolves fully, solution is crossed the DAD-1 that has handled and is removed acid resin, with 95% an amount of methanol-eluted fractions, collects and merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 28kg of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Embodiment 24:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=7% Folium Ginkgo extract 30kg, after acetone with 30% dissolves fully, solution is crossed the DAD-1 that handled and is removed acid resin, and the acetone wash-out with an amount of 30% is collected also merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 27.9kg of Folium Ginkgo terpene lactones 〉=7%.Resin is reused after diverse ways is handled.
Embodiment 25:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=9% Folium Ginkgo extract 30kg, after acetone with 70% dissolves fully, solution is crossed the DAD-1 that handled and is removed acid resin, and the acetone wash-out with an amount of 70% is collected also merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 28.9kg of Folium Ginkgo terpene lactones 〉=8.5%.Resin is reused after diverse ways is handled.
Embodiment 26:
Get flavonol glycosides 〉=24%, Folium Ginkgo terpene lactones 〉=6% Folium Ginkgo extract 30g, after acetone with 95% dissolves fully, solution is crossed the DAD-1 that handled and is removed acid resin, and the acetone wash-out with an amount of 95% is collected also merging effluent liquid and elutriant, at≤75 ℃ of concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=25%, the Folium Ginkgo extract 28g of Folium Ginkgo terpene lactones 〉=6%.Resin is reused after diverse ways is handled.
Claims (8)
1. the preparation method of an extractive of low acidic gingko leaves, it mainly comprises the following steps: with the Ginkgo Leaf to be raw material:
(a) with 40%-95% ethanol or 40%-100% methyl alcohol or 40%-100% acetone extraction;
(b) get extracting solution and concentrate recovery ethanol or methyl alcohol or acetone;
(c) concentrated solution dilutes cold-1 ℃ to the 20 ℃ sedimentations of going but;
(d) supernatant liquor is crossed the absorption of styrene tyle macroporous adsorption resin post;
(e) with alcohols or acetone soln wash-out;
(f) elutriant is crossed the absorption of DAD-1 deacidification resin column;
(g) with alcohols or acetone soln wash-out;
(h) effluent liquid and elutriant concentrate drying;
2. the preparation method of extractive of low acidic gingko leaves according to claim 1, it is characterized in that: step (e) is a wash-out, eluent is methyl alcohol or ethanol or acetone, concentration 30%-95%.
3. the preparation method of extractive of low acidic gingko leaves according to claim 1 is characterized in that: step (e) is gradient elution, and eluent is methyl alcohol or ethanol or acetone, and wash-out concentration is 0%-30% for the first time, and wash-out concentration is 40%-95% for the second time.
4. the preparation method of extractive of low acidic gingko leaves according to claim 3, it is characterized in that: the eluent of step (g) is methyl alcohol or ethanol or acetone, and its concentration is 30%-95%.
5. the preparation method of extractive of low acidic gingko leaves according to claim 4 is characterized in that: the thinner that the described concentrated solution dilution of step (c) is adopted is water or purified water.
6. the preparation method of extractive of low acidic gingko leaves according to claim 5 is characterized in that: step (c) is concentrated solution dilution back roughing out, redilution, cooling natural subsidence.
7. the preparation method of extractive of low acidic gingko leaves according to claim 6 is characterized in that: step (a) is extracted for dipping, and temperature range is a normal temperature to 80 ℃.
8. the method for preparing Folium Ginkgo extract according to claim 7 is characterized in that: step (h) elutriant thickening temperature is less than 75 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031148263A CN1318440C (en) | 2003-01-08 | 2003-01-08 | Preparation method of low-acid ginkgo leaf extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031148263A CN1318440C (en) | 2003-01-08 | 2003-01-08 | Preparation method of low-acid ginkgo leaf extract |
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510060376 Division CN1733269A (en) | 2003-01-08 | 2003-01-08 | Drop pill made from root rhizome and herb of common lamiophlomis and process for preparing the same |
| CN 200510097920 Division CN1795879A (en) | 2003-01-08 | 2003-01-08 | Method for preparing extractive of low acidic gingko leaves |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1515582A CN1515582A (en) | 2004-07-28 |
| CN1318440C true CN1318440C (en) | 2007-05-30 |
Family
ID=34239418
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031148263A Expired - Fee Related CN1318440C (en) | 2003-01-08 | 2003-01-08 | Preparation method of low-acid ginkgo leaf extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1318440C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101175506B (en) * | 2005-05-03 | 2012-06-06 | 威玛舒培博士两合公司 | Method for preparing a ginkgo extract having a reduced content of 4'-o-methyl pyridoxine and/or biflavones |
| CN100421680C (en) * | 2005-08-10 | 2008-10-01 | 北京星昊医药股份有限公司 | Extractive of ginkgo tree leaves, prepn. method and application thereof |
| CN101785559B (en) * | 2009-12-29 | 2012-08-08 | 孙羽菡 | Processing method utilizing gingko to prepare gingko detoxifying powder and co-generate crude ginkgo phenolic acid extract |
| CN102078342A (en) * | 2010-12-22 | 2011-06-01 | 天津泰阳制药有限公司 | Preparation method of water-soluble ginkgo biloba extract (GBE) |
| CN102091103B (en) * | 2011-01-25 | 2012-09-05 | 江苏九久环境科技有限公司 | Method for preparing gingko extract with low acid number by ultrasonic extraction |
| CN102614229B (en) * | 2012-04-25 | 2015-04-08 | 江苏神龙药业有限公司 | Method for removing ginkgolic acid from ginkgo biloba extract |
| CN102728096B (en) * | 2012-07-10 | 2014-06-11 | 江苏惠康生物有限公司 | Edulcoration method of ginkgo leaf extraction process |
| CN104208108A (en) * | 2014-09-19 | 2014-12-17 | 邹其芃 | Method for effectively separating low-acid gingko leaf extract |
| CN105596382A (en) * | 2016-01-14 | 2016-05-25 | 重庆万物春生制药有限公司 | Extraction process of ginkgo biloba extract |
| CN106074631B (en) * | 2016-07-27 | 2019-11-15 | 晨光生物科技集团股份有限公司 | A kind of low ginkgoic acid low ash divides the industrialized preparing process of ginkgo biloba p.e |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116532A (en) * | 1994-08-11 | 1996-02-14 | 邓忠元 | Process for producing extract of gingko leaves |
| CN1129218A (en) * | 1995-11-15 | 1996-08-21 | 庚朋 | Process for extracting total flavone from ginkgo leaf |
| CN1374300A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Resin process of eliminating ginkgolic acid from gingko leaf extractive |
| CN1374301A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Process of eliminating tannic acid from ginkgo leaf extractive |
| CN1374303A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Production process of water soluble ginkgo leaf extractive |
-
2003
- 2003-01-08 CN CNB031148263A patent/CN1318440C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116532A (en) * | 1994-08-11 | 1996-02-14 | 邓忠元 | Process for producing extract of gingko leaves |
| CN1129218A (en) * | 1995-11-15 | 1996-08-21 | 庚朋 | Process for extracting total flavone from ginkgo leaf |
| CN1374300A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Resin process of eliminating ginkgolic acid from gingko leaf extractive |
| CN1374301A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Process of eliminating tannic acid from ginkgo leaf extractive |
| CN1374303A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Production process of water soluble ginkgo leaf extractive |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1515582A (en) | 2004-07-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6117431A (en) | Method for obtaining an extract from ginkgo biloba leaves | |
| CN1318440C (en) | Preparation method of low-acid ginkgo leaf extract | |
| CN103665059B (en) | A kind of natural crocin extraction separation method and the preparation of blood lipid-lowering medicine thereof | |
| CN112472727B (en) | Method for co-producing ginkgo leaf extract, terpene lactone and shikimic acid | |
| CN107556283A (en) | A kind of process of the extraction of the efficient low-consume from grape pip OPC | |
| JP3808494B2 (en) | Method for producing high content of proanthocyanidins | |
| CN107115367B (en) | Fermentation production method for efficiently extracting flavone from ginkgo leaves | |
| CN102078341B (en) | High-purity ginkgo flavone and composition thereof | |
| CN103251659B (en) | Preparation method of ginkgo leaf essence | |
| CN107158048A (en) | A kind of high efficiency from ginkgo leaf extracts flavones and the method for being converted into glucoside type flavone | |
| CN100362011C (en) | Preparation method of ginkgo leaf extract | |
| CN105616477A (en) | Method for purifying polyphenol in lonicera edulis | |
| JP2996716B2 (en) | How to get ginkgo biloba extract | |
| CN104945450A (en) | Method for extracting stibene glucoside from vines of multiflower knotweeds | |
| CN108552370A (en) | A method of extraction tea polyphenols | |
| CN107213180A (en) | A kind of separating and extracting process of pseudo-ginseng flavones | |
| CN112043733A (en) | Production method of water-soluble ginkgo leaf extract | |
| CN108210554B (en) | Method for separating and purifying alcohol-soluble total flavonoids from liquorice | |
| CN111187669A (en) | Extraction method of magnolia flower volatile oil | |
| NL2028620B1 (en) | Method for extracting total flavonoids from lycium chinese leaves | |
| CN112159382B (en) | Method for efficiently preparing active oligomeric proanthocyanidins from physiological fruit drop of litchi | |
| DE2358434A1 (en) | METHOD FOR PURIFYING VEGETABLE FLAVONE EXTRACTS | |
| CN1379026A (en) | Process for preparing gingko leaf extract | |
| CN1362252A (en) | Method of eliminating gingkolic acid from gingko extract | |
| CN105541938B (en) | The method that macroporous adsorbent resin method prepares natural aucubin is increased using UF membrane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070530 Termination date: 20220108 |