CN101278989B - Method for extracting Thalictrum aquilegifolium total alkaloids and total saponins from Thalictrum aquilegifolium - Google Patents
Method for extracting Thalictrum aquilegifolium total alkaloids and total saponins from Thalictrum aquilegifolium Download PDFInfo
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Abstract
The invention relates to a method for extracting Thalictrum squarrosum total alkaloids and total saponins from grass of meadow rue, pertaining to biological and pharmaceutical technical field. The invention discloses the method for simultaneously preparing extracts of total alkaloids and total saponins from grass of meadow rue. The invention uses an absorption resin for absorbing the total alkaloids and the total saponins from grass of meadow rue, an organic solvent or the water solution thereof is utilized to desorb the absorption resin; then an ion exchange resin is used for selectively absorbing alkaloids from grass of meadow rue extract, thus obtaining the saponins from eluate. The method of the invention enhances the extracting efficiency of effective group of components from grass of meadow rue, avoids the loss of effective components, and saves the sources; the content of the extract of total alkaloids purified by using the method is higher than 50 percent, and the content of the extract of total saponins is higher than 30 percent.
Description
Technical field
The invention belongs to the biological medicine technology field.Be specifically related to a kind of preparation method of Thalictrum aquilegifolium L. var. sibiricum Regel bio-extract.
Background technology
The effects such as that Ranunculaceae Thalictrum (Thalictrum L.) plant has is anticancer, anti-inflammation, antiviral, arrhythmia, malaria, immunomodulating, blood pressure lowering, heat-clearing and toxic substances removing, analgesia, diuresis.Thalictrum spp is medicinal extensively at national folk, China has 67 kinds of these platymisciums to use at 15 ethnic drugs, it is the important component part that numerous ethnic drugs such as Tibetan medicine, mongolian medicine are used, mainly concentrate on southwest, owing to thering is unique geography and climatic environment, this platymiscium of China is over half is endemic species, and aboundresources.Containing alkaloids composition and triterpenoid saponins in the Thalictrum aquilegifolium L. var. sibiricum Regel plant, is medicinal active ingredient main in Thalictrum aquilegifolium L. var. sibiricum Regel, has the effects such as anticancer, antibacterial, blood pressure lowering, makes Thalictrum aquilegifolium L. var. sibiricum Regel extensive use in medicine, health product, cosmetics etc.
At present, the research of Thalictrum aquilegifolium L. var. sibiricum Regel is only limited to the research of Thalictrum aquilegifolium L. var. sibiricum Regel compound structure, [Zhang Xiantao Wang Hao etc., the chemical composition of East China Thalictrum aquilegifolium L. var. sibiricum Regel, China Medicine University's journal, 2007,38 (1): 21-24.] a kind of chromatography method is disclosed for extracting the Thalictrum aquilegifolium L. var. sibiricum Regel compound, but the method can't for the production of; [the technical study of macroporous adsorbent resin separation and purification Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids of openly knowing clearly such as Cai Yingfan, Chinese patent medicine, 2007,29 (11): 1609-1611.], the purpose of these methods is in order to extract alkaloid from Thalictrum aquilegifolium L. var. sibiricum Regel, yet adopt said method extracting the alkaloidal while also out by saponin extraction simultaneously, there is no the process of further the alkaloids composition being separated with saponin component in the extracting method of prior art, so the method imperfection, DNA purity is not high, the waste resource.At present, having no report in open source literature extracts simultaneously and separates the method for preparing Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and total saponins.
Summary of the invention
Technical problem to be solved by this invention is, also extract saponin when in the prior art extracting method, Thalictrum aquilegifolium L. var. sibiricum Regel being carried out to the alkaloid extraction, DNA purity is not high, the defect of waste resource, provide a kind of low cost, high yield, be suitable for the Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids of suitability for industrialized production and the preparation method of total saponins.Thalictrum aquilegifolium L. var. sibiricum Regel alkaloid compound and saponins compound are separated from Thalictrum aquilegifolium L. var. sibiricum Regel to Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and total saponins class extract that then further separation and Extraction purity is high, impurity content is few simultaneously.
The present invention includes following steps:
(1) add polar organic solvent in Thalictrum aquilegifolium L. var. sibiricum Regel, mix homogeneously, filtration, decompression and solvent recovery, vacuum concentration extract the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract; (2) add suitable quantity of water in the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract, and stir into suspension, make suspension proportion reach 1.0～1.2; (3) suspension is adsorbed by the adsorbent resin detached dowel, with organic solvent, in room temperature to 50 ℃, the adsorbent resin detached dowel is resolved, or water is resolved at 40～100 ℃, the desorbed solution consumption is 2-6 resin volume doubly, and decompression and solvent recovery, vacuum concentration obtain the Thalictrum extract after purification; (4) add in Thalictrum extract and make suspension proportion reach 1.0～1.2 water, stir into suspension, suspension is passed through to cation exchange resin column, collection is by the effluent of cation exchange resin column, control temperature concentrated effluent under 40～80 ℃, obtain total saponins class extract; (5) adopt 1～10% NaOH aqueous solution or aqueous solutions of organic solvent cation exchange resin column to be resolved to the desorbed solution that obtains ion exchange, with hydrochloric acid or sulfuric acid acidation desorbed solution, make it reach pH=5～7, under 40～80 ℃ of temperature conditions, it is concentrated, obtained total alkaloids class extract.Polar organic solvent described in step (1) comprises the mixed solvent that methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol, acetone or above-mentioned solvent form by a certain percentage, or the acidity or the basic solvent that by these solvents and acid, alkali, salt, are made into.Can preferentially select ethanol or acetone as polar organic solvent.In leaching process, the ratio rate of charge is raw material: solvent=1: 1～20; The condition of decompression and solvent recovery is-0.05～0.09Mpa, 50～65 ℃.The water that the desorbed solution that the adsorbent resin detached dowel is resolved is ethanol, propanol, methanol, acetone or 40～100 ℃.The aqueous solutions of organic solvent that cation exchange resin column is resolved is ethanol, propanol, methanol, acetone.
The invention discloses the extraction separation method of total alkaloids and total saponins in a kind of Thalictrum aquilegifolium L. var. sibiricum Regel, technique is simple, cost is low, it is little to lose, product quality is high, non-environmental-pollution.Improve the extraction efficiency of active component group in the Thalictrum aquilegifolium L. var. sibiricum Regel, avoided the loss of effective ingredient.The resin structure that the present invention uses is stable, and contamination resistance is strong, is easy to regeneration, and total alkaloids in Thalictrum aquilegifolium L. var. sibiricum Regel and total saponins are had to very high selectivity.Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and the total saponin extracts purity extracted are high, have improved the extraction efficiency of active component group in the Thalictrum aquilegifolium L. var. sibiricum Regel, have avoided the loss of effective ingredient, economize on resources.The total alkaloid content of use this method purification>50%, the content of total saponins>30%.
The specific embodiment
From Thalictrum aquilegifolium L. var. sibiricum Regel, extract total alkaloids and total saponins the concrete steps of being separated are as follows:
(1) the Thalictrum aquilegifolium L. var. sibiricum Regel herb is broken into to coarse powder or be cut into the 2-3cm quarter butt with pulverizer and put into container, adding polar organic solvent to stir becomes mixture, and rate of charge can be raw material: solvent=1: 1～20; Backflow 1～10h under room temperature (can meet-10～70 ℃ of temperature) (hour) extract, or water logging is extracted; Described polar organic solvent comprises the mixed solvent that methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol, acetone or above-mentioned solvent form by a certain percentage, or the acidity or the basic solvent that by these solvents and acid, alkali, salt, are made into.Can preferentially select ethanol or acetone as polar organic solvent.Said mixture is extracted 1～3 time, and merge extractive liquid,, filter extracting solution, under-0.05～0.09Mpa, 50～65 ℃ of conditions, to extracting solution carry out decompression and solvent recovery, vacuum concentration becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract;
(2) the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water, it is stirred into to suspension, make suspension proportion reach 1.0～1.2;
(3) adopt adsorbent resin to be separated suspension, the suspension of above-mentioned steps (2) gained is passed through to the adsorbent resin detached dowel, adsorbent resin can be HPD100, HPD300, HPD700, D101, AB-8, XDA-1, H-20, one or more hybrid resins in the HZ-841 model, the suspension flow velocity can be controlled in 3～5ml/min, under room temperature (maximum temperature can be controlled in 50 ℃) condition, (comprise ethanol with organic solvent, propanol, methanol, acetone and other organic solvent) as desorbed solution, above-mentioned adsorbent resin is resolved, or resolved as solvent with 40～100 ℃ of water, or adopt the mixed liquor of water and organic solvent to resolve, flow velocity can be controlled in 0.2-0.6ml/min, the 2-6 that the desorbed solution consumption is the adsorbent resin volume doubly, under-0.05～0.09Mpa, 50～65 ℃ of conditions, after decompression and solvent recovery, vacuum concentration purification, obtain Thalictrum extract.
(4) ion exchange adds suitable quantity of water in Thalictrum extract, and it is stirred into to suspension, makes suspension proportion reach 1.0～1.2; By suspension, by cation exchange resin column, (can be 001 * 7, TS-92, TS-80, D113, DK110, one or more hybrid resins in 724 models) carry out ion exchange absorption, controllable flow speed is at 0.2-0.6ml/min, through ion exchange, alkaloids substance is adsorbed on resin column, and saponins compound flows out with effluent; Under 40～80 ℃ of temperature conditions, effluent is concentrated, obtained total saponins class extract;
(5) with 1～10% NaOH aqueous solution or aqueous solutions of organic solvent (comprising ethanol, propanol, methanol, acetone and other organic solvent) as desorbed solution, ion exchange resin to above-mentioned steps (4) is resolved, flow velocity can be controlled in 0.2-0.6ml/min, the desorbed solution consumption is 2-6 resin volume doubly, obtains the desorbed solution that contains alkaloid compound; , desorbed solution is concentrated under 40～80 ℃ of temperature conditions to pH=5～7 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.
Below by specific embodiment, the invention will be further described.
Embodiment 1
Take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L water to stir, control temperature in the time of 70 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to 3 times to be extracted, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration.The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.20, adopt HPD700 model macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, wash away impurity with the water (V/V) of 2 times of amount of resin, then use the methanol that 5 times of amount of resin (V/V) concentration is 50% to be resolved, collect desorbed solution, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract.Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.15, adopt 001 * 7 model ion exchange resin, enrichment is adsorbed to saturated, adds the water (V/V) of 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, use again the NaOH-ethanol parsing that 5 times of amount of resin (V/V) concentration is 2% to stay the alkaloids substance on resin column, collect desorbed solution, reclaim under reduced pressure effluent at 65 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 50 ℃ of temperature conditions to pH=5.6 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.Measuring the Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloid extractive content is 59%; Total saponin extracts content is 35%.
Embodiment 2
Take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L 50% ethanol to stir, control temperature at 85 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to reflux, extract, 3 times, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration.The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.11, adopt AB-8 model macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, wash away impurity with the water (V/V) of 2 times of amount of resin, then use the ethanol that 4 times of amount of resin (V/V) concentration is 70% to be resolved, collect desorbed solution, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract.Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.02, adopt TS-80 model ion exchange resin, enrichment is adsorbed to saturated, adds the water (V/V) of 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, use again the ammonia that 5 times of amount of resin (V/V) concentration is 10%-methanol to resolve and stay the alkaloids substance on resin column, collect desorbed solution, reclaim under reduced pressure effluent at 58 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 55 ℃ of temperature conditions to pH=6.8 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.Measuring the Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloid extractive content is 52%; Total saponin extracts content is 40%.
Embodiment 3
Take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L 70% ethanol to stir, control temperature at 88 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to reflux, extract, 3 times, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration.The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.09, adopt XDA-1, AB-8 (1: 1) mixed type macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, wash away impurity with the water (V/V) of 2 times of amount of resin, then use the ethanol that 5 times of amount of resin (V/V) concentration is 50% to be resolved, collect desorbed solution, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract.Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.11, adopt TS-92 model ion exchange resin, enrichment is adsorbed to saturated, adds the water (V/V) of 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, use again the ammonia that 5 times of amount of resin (V/V) concentration is 3%-acetone to resolve and stay the alkaloids substance on resin column, collect desorbed solution, reclaim under reduced pressure effluent at 56 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 55 ℃ of temperature conditions to pH=5.8 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.Measuring the Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloid extractive content is 62%; Total saponin extracts content is 31%.
Embodiment 4
Take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L 70% methanol to stir, control temperature at 85 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to reflux, extract, 3 times, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration.The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.17, adopt HZ-841 model macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, wash away impurity with the water (V/V) of 2 times of amount of resin, then use the acetone that 4 times of amount of resin (V/V) concentration is 50% to be resolved, collect desorbed solution, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract.Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.16, adopt DK110 model ion exchange resin, enrichment is adsorbed to saturated, add the water (V/V) of 3 times of amount of resin to be washed, collect the effluent containing saponins compound, use again the ethamine that 5 times of amount of resin (V/V) concentration is 10%-methanol mixed the solvent analysis to stay the alkaloids substance on resin column, collect desorbed solution, reclaim under reduced pressure effluent at 61 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 57 ℃ of temperature conditions to pH=6.2 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.Measuring the Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloid extractive content is 54%; Total saponin extracts content is 37%.
Claims (4)
1. a method of extracting Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and total saponins from Thalictrum aquilegifolium L. var. sibiricum Regel, it is characterized in that, comprise the steps: to take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L water to stir, control temperature in the time of 70 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to 3 times to be extracted, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration; The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.20, adopt HPD700 model macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, the washing decontamination that is 2 times of amount of resin with volume, then be that the methanol that 5 times of amount of resin concentration are 50% is resolved with volume, desorbed solution collected, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract; Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.15, adopt 001 * 7 model ion exchange resin, enrichment is adsorbed to saturated, adds the water that volume is 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, with volume, be that the alkaloids substance on resin column is stayed in the NaOH-ethanol parsing that 5 times of amount of resin concentration are 2% again, collect desorbed solution, reclaim under reduced pressure effluent at 65 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 50 ℃ of temperature conditions to pH=5.6 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.
2. a method of extracting Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and total saponins from Thalictrum aquilegifolium L. var. sibiricum Regel, it is characterized in that, comprise the steps: to take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L50% ethanol to stir, control temperature at 85 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to reflux, extract, 3 times, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration; The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.11, adopt AB-8 model macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, the washing decontamination that is 2 times of amount of resin with volume, then be that the ethanol that 4 times of amount of resin concentration are 70% is resolved with volume, desorbed solution collected, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract; Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.02, adopt TS-80 model ion exchange resin, enrichment is adsorbed to saturated, adds the water that volume is 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, with volume, be that 5 times of amount of resin concentration ammonia-methanol that is 10% is resolved and stayed the alkaloids substance on resin column again, collect desorbed solution, reclaim under reduced pressure effluent at 58 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 55 ℃ of temperature conditions to pH=6.8 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.
3. a method of extracting Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and total saponins from Thalictrum aquilegifolium L. var. sibiricum Regel, it is characterized in that, comprise the steps: to take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L70% ethanol to stir, control temperature at 88 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to reflux, extract, 3 times, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration; The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.09, adopt XDA-1, AB-8 mixed type macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, the washing decontamination that is 2 times of amount of resin with volume, then be that the ethanol that 5 times of amount of resin concentration are 50% is resolved with volume, desorbed solution collected, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract; Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.11, adopt TS-92 model ion exchange resin, enrichment is adsorbed to saturated, adds the water that volume is 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, with volume, be that 5 times of amount of resin concentration ammonia-acetone that is 3% is resolved and stayed the alkaloids substance on resin column again, collect desorbed solution, reclaim under reduced pressure effluent at 56 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 55 ℃ of temperature conditions to pH=5.8 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.
4. a method of extracting Thalictrum aquilegifolium L. var. sibiricum Regel total alkaloids and total saponins from Thalictrum aquilegifolium L. var. sibiricum Regel, it is characterized in that, comprise the steps: to take the dry herb powder of Thalictrum aquilegifolium L. var. sibiricum Regel 1Kg, add 10L70% methanol to stir, control temperature at 85 ℃, the Thalictrum aquilegifolium L. var. sibiricum Regel powder is carried out to reflux, extract, 3 times, each extraction time interval 1h, merge extractive liquid,, filter, filtrate, under-0.05～0.09Mpa, 50～65 ℃ of conditions, becomes the Thalictrum aquilegifolium L. var. sibiricum Regel crude extract through decompression and solvent recovery, vacuum concentration; The Thalictrum aquilegifolium L. var. sibiricum Regel crude extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.17, adopt HZ-841 model macroporous adsorbent resin to be adsorbed suspension, enrichment is adsorbed to saturated, the washing decontamination that is 2 times of amount of resin with volume, then be that the acetone that 4 times of amount of resin concentration are 50% is resolved with volume, desorbed solution collected, control temperature at 50～65 ℃ of decompression and solvent recoveries, residue dried obtains Thalictrum extract; Thalictrum extract is added to suitable quantity of water and stir into suspension, make suspension proportion reach 1.16, adopt DK110 model ion exchange resin, enrichment is adsorbed to saturated, adds the water that volume is 3 times of amount of resin to be washed, and collects the effluent containing saponins compound, with volume, be that 5 times of amount of resin concentration are 10% ethamine-methanol mixed the solvent analysis is stayed the alkaloids substance on resin column again, collect desorbed solution, reclaim under reduced pressure effluent at 61 ℃ of temperature, obtain the Thalictrum aquilegifolium L. var. sibiricum Regel total saponin extracts; , desorbed solution is concentrated under 57 ℃ of temperature conditions to pH=6.2 with hydrochloric acid or sulfuric acid acidation, obtained total alkaloids class extract.
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| CN102697879B (en) * | 2012-06-27 | 2014-03-05 | 耐珀（北京）科技有限公司 | Application of Thalictrum robustum Maxim. in extracting drug for treating human cardiovascular diseases |
| CN102716203B (en) * | 2012-06-27 | 2014-06-18 | 耐珀（北京）科技有限公司 | Thalictrum robustum maxim extract for treating hypertension and application of thalictrum robustum maxim extract |
| CN102716202B (en) * | 2012-06-27 | 2014-03-05 | 中国医学科学院药用植物研究所 | Method for extracting medicine for treating human cardiovascular diseases from thalictrum robustum |
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| CN1267670A (en) * | 2000-03-23 | 2000-09-27 | 肖培根 | Two aporphine-benzyl isoquinoline compounds with antineoplastic activity |
| CN1285354A (en) * | 1999-08-19 | 2001-02-28 | 广州市海科生物技术有限公司 | Thalictrum acutifolium thalicrine having anti-tumour phological activity and extration method thereof |
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2008
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|---|---|---|---|---|
| CN1285354A (en) * | 1999-08-19 | 2001-02-28 | 广州市海科生物技术有限公司 | Thalictrum acutifolium thalicrine having anti-tumour phological activity and extration method thereof |
| CN1267670A (en) * | 2000-03-23 | 2000-09-27 | 肖培根 | Two aporphine-benzyl isoquinoline compounds with antineoplastic activity |
Non-Patent Citations (3)
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| 张蔚君等.大孔吸附树脂在中草药有效成分提纯中的应用及其影响因素.《空军总医院学报》.2006,第22卷(第2期), * |
| 江邦和等.离子交换与吸附树脂在中药有效成分提取中的应用.《离子交换与吸附》.2001,第17卷(第4期), * |
| 蔡应繁等.大孔吸附树脂分离纯化唐松草总生物碱的工艺研究.《中成药》.2007,第29卷(第11期), * |
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