CN101619062B - Natural fibrauretine crystal and macroporous adsorbent resin preparation method thereof - Google Patents
Natural fibrauretine crystal and macroporous adsorbent resin preparation method thereof Download PDFInfo
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- CN101619062B CN101619062B CN2009100542841A CN200910054284A CN101619062B CN 101619062 B CN101619062 B CN 101619062B CN 2009100542841 A CN2009100542841 A CN 2009100542841A CN 200910054284 A CN200910054284 A CN 200910054284A CN 101619062 B CN101619062 B CN 101619062B
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Abstract
The invention relates to a fibrauretine crystal extracted from calamus margaritae roots or stems and a preparation method thereof. The preparation method of the fibrauretine crystal is as follows: alkaloid components contained in the calamus margaritae roots or stems are extracted by an organic solvent, an extraction solution is decompressed and concentrated, concentrated materials are separated and purified by macroporous adsorbent resin so as to obtain an alkaloid extractive containing fibrauretine, and the alkaloid extractive continues to be purified by the macroporous adsorbent resin and then recrystallized so as to obtain the fibrauretine crystal. The total content of fibrauretine 1 and fibrauretine 2 contained in the fibrauretine crystal can achieve more than 81 percent. The invention provides the efficient, simple and convenient preparation method and is suitable for large-scale production.
Description
[technical field]
The present invention relates to a kind of effective ingredient in Chinese extractive technique field.More specifically, the present invention relates to a kind of fibrauretine crystal, also relate to the method that adopts the macroporous adsorbent resin method to prepare said fibrauretine crystal.
[background technology]
Herba fibraureae recisae has another name called Root or stem of Wintergreen Barberry, huangteng, is root and the stem of menispermaceae plant herba fibraureae recisae.Cold in nature, sweet-bitter flavor.The herba fibraureae recisae vegeto-alkali is a kind of vegeto-alkali that from herba fibraureae recisae, extracts, and root of herba fibraureae recisae and stem contain palm leaf coculine, neprotin, Berberine, and other contains fibranine, fibraminine, Columbin and sterol, has effects such as clearing heat and detoxicating, that anti-inflammatory is antibacterial.Wherein Fibrauretin is widely used in field of medicaments such as gynecological inflammation, enteritis, respiratory tract and urinary tract infection, surgical infection, eye conjunctivitis.
Macroporous adsorbent resin is one type of cross-linked polymer that does not contain ion-exchange group, and physico-chemical property is stable, is insoluble to acid, alkali and organic solvent, and organism is had concentrated, centrifugation and do not receive the interference of inorganic salts, strong ion and low molecular compound.Macroporous adsorbent resin through physical adsorption selectively adsorb organic compound matter reach the purpose of separate purifying.According to the surface properties of resin, can be divided into three types of nonpolar, Semi-polarity and polarity.
At present, the separation purification method of Chinese medical extract can be divided three classes substantially: solvent extration, supercritical fluid extraction, column chromatography.The organic solvent extractionprocess that adopts obtains to contain the more of herba fibraureae recisae alkaloid extraction thing; But all need use multiple inflammable and explosive organic solvent, industrial equipments is required height, complicated operating process; Weak points such as product yield is not high, and waste liquid exhaust emission environment is serious.The weak point of supercritical fluid extraction is that the plant and instrument cost is high, and energy consumption is serious.The main drawback of column chromatography is that silica gel can not be regenerated, and production cost is high.Therefore, still also need a kind of safe, pollution-free, low operation cost, Chinese medical extract separation purification method that the recovery is high of extracting, the inventor has accomplished the present invention finally through a large amount of experimental studies for this reason.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of fibrauretine crystal.
Another object of the present invention provides a kind of method that adopts the macroporous adsorbent resin method to prepare said fibrauretine crystal.
[technical scheme]
The present invention realizes through following technical proposals.
The present invention relates to a kind of employing macroporous adsorbent resin method and prepare natural Fibrauretin crystalline method.The step of this method is following:
(1) get dried herba fibraureae recisae root or stem powder, with an organic solvent the weight ratio 8-10 with said organic solvent and said herba fibraureae recisae root or stem powder at room temperature extracted 1.5-2.5 hour, repeated to extract 2-3 time; United extraction liquid; Carry out concentrating under reduced pressure then, reclaim organic solvent, obtain enriched material;
(2) enriched material that obtains of step (1) uses 10%-20% (V/V) aqueous ethanolic solution to dissolve with the weight ratio 1 of said enriched material and said aqueous ethanolic solution: 2-4; Mix with macroporous adsorbent resin then, the dry weight of said polymeric adsorbent is dried herba fibraureae recisae root or stem weight 8-10 a times, is incorporated as the water of 10 times of said aqueous ethanolic solution volumes then; Install on the described macroporous adsorptive resins after stirring 2-3h; Water wash to elutant colourless after, use the organic solvent wash-out again, said volume of organic solvent is a 2-4 times of column volume; Its flow velocity is 0.5-1 times of column volume/h; The elutriant that obtains carries out concentrating under reduced pressure, reclaims organic solvent, obtains being brown buttery herba fibraureae recisae alkaloid extract;
(3) the herba fibraureae recisae alkaloid extract that step (2) is obtained uses the dissolving of 90%-98% (V/V) aqueous ethanolic solution with the weight ratio 1 of said extract and said aqueous ethanolic solution: 2-4; Mix with described macroporous adsorbent resin then; The dry weight of described polymeric adsorbent is 8-10 a times of said herba fibraureae recisae alkaloid extract weight, is incorporated as the water of 10 times of said aqueous ethanolic solution volumes then, joins on the described macroporous adsorptive resins behind the stirring 2-3h; Water wash to elutant be colourless after; Earlier use the non-polar organic solvent wash-out, use the polar organic solvent wash-out again, the volume of said polar organic solvent is a 2-4 times of column volume; Its flow velocity is 0.5-1 times of column volume/h, collects the polar organic solvent elutriant;
(4) the polar organic solvent elutriant that step (3) is obtained carries out concentrating under reduced pressure; Reclaim organic solvent; The enriched material that obtains is used the recrystallization organic solvent dissolution, at temperature 25-60 ℃ of vibration 15-25min, leaves standstill crystallization then; Recrystallization is carried out in the crystallization that obtains in the recrystallization organic solvent, obtain being the flaky Fibrauretin vegeto-alkali of leaflet crystallized product.
According to a preferred embodiment of the invention a, be one or more organic solvents that are selected from ethanol, methyl alcohol, acetone or ETHYLE ACETATE in step (1) with the organic solvent described in (2).
According to another preferred embodiment of the invention, be HPD series macroporous adsorbent resin 100 or 300 models or the close macroporous adsorbent resin of its polarity at the macroporous adsorbent resin described in the step (2).
According to another preferred embodiment of the invention, be one or more non-polar organic solvents that are selected from sherwood oil, ether or normal hexane at the non-polar organic solvent described in the step (3).
According to another preferred embodiment of the invention, be HPD series macroporous adsorbent resin 500 or 600 models or the close macroporous adsorbent resin of its polarity at the macroporous adsorbent resin described in the step (3).
According to another preferred embodiment of the invention, described concentrating under reduced pressure temperature 30-50 ℃ with vacuum tightness 0.1-0.5MPa condition under carry out.
According to another preferred embodiment of the invention, the said polar solvent as elutriant is ethanol, methyl alcohol, acetone or the ETHYLE ACETATE of concentration greater than 95% (V/V) in the step (3).
According to another preferred embodiment of the invention, described recrystallization organic solvent is one or more solvents that are selected from sherwood oil, ether or normal hexane.
The present invention relates to the Fibrauretin crystallized product that adopts above-mentioned preparation method to obtain, it is characterized in that this product contains 81% above fibranine and fibraminine.
Below the present invention will be described in more detail.
The present invention adopts following technical scheme to prepare the Fibrauretin crystallization: get dried herba fibraureae recisae root or stem, pulverize, with organic solvent extraction 2-3 time; United extraction liquid and concentrating under reduced pressure, the enriched material that obtains is used dissolve with ethanol, mixes with polymeric adsorbent then; Add entry again, be added to after the stirring on the macroporous adsorbent resin, the polar organic solvent wash-out is used in first water flushing again; Elutriant carries out concentrating under reduced pressure, obtains the herba fibraureae recisae alkaloid extract.This extract with aqueous ethanolic solution dissolving, mixes with polymeric adsorbent more then, adds entry again, is being added to after the stirring on the macroporous adsorbent resin, washes with big water gaging again, and is first then with non-polar organic solvent, carry out wash-out with polar organic solvent again.Elutriant carries out concentrating under reduced pressure, and the enriched material that obtains obtains expecting the crystallization of product Fibrauretin with organic solvent dissolution post crystallization twice.
Particularly, the preparation process of fibrauretine crystal of the present invention is following:
(1) get dried herba fibraureae recisae root or stem powder, with an organic solvent the weight ratio 8-10 with said organic solvent and said herba fibraureae recisae root or stem powder at room temperature extracted 1.5-2.5 hour, repeated to extract 2-3 time; United extraction liquid; Carry out concentrating under reduced pressure then, reclaim organic solvent, obtain enriched material.
Herba fibraureae recisae root or stem need carry out drying treatment before processing treatment, usually in loft drier, under 50 ℃-75 ℃ of temperature, carried out dry 2-3 hour.Described loft drier is the drying plant that common Chinese medicinal materials processing is used.Herba fibraureae recisae root or stem generally are being lower than 1.0 weight % through the water cut after the drying treatment.
Dried herba fibraureae recisae root or stem re-use in the Chinese medicinal materials manufacture field normally used disintegrating apparatus and pulverize, and the granularity of pulverizing herba fibraureae recisae root or stem generally is the 20-200 order.Certainly, the granularity of herba fibraureae recisae root or stem is not very crucial, and the herba fibraureae recisae root or the stem that surpass this size range also can use, and therefore, these size ranges do not exceed protection scope of the present invention.
In the present invention, organic solvent should be appreciated that it is a kind of organic solvent that can the herba fibraureae recisae vegeto-alkali be extracted from its herba fibraureae recisae root or stem, and these organic solvents are a kind of volatile, and its residue also can not produce the organic solvent of adverse consequences to tobacco product.
In the present invention, described organic solvent is a kind of organic solvent that is selected from ethanol, methyl alcohol, acetone or ETHYLE ACETATE.In the present invention, described ethanol, methyl alcohol generally are aqueous ethanolic solution, methanol aqueous solution.
Preferably, described organic solvent is aqueous ethanolic solution or acetone.
More preferably, described organic solvent is an aqueous ethanolic solution.
In the present invention, described organic solvent concentration is more than 50% (V/V), and its add-on is dried herba fibraureae recisae root or stem powder weight 8-10 a times.
Described organic solvent need reclaim after extraction step is accomplished, and the distillation method that adopts the technician in present technique field to know usually reclaims.
(2) enriched material that obtains of step (1) uses 10%-20% (V/V) aqueous ethanolic solution to dissolve with the weight ratio 1 of said enriched material and said aqueous ethanolic solution: 2-4; Mix with macroporous adsorbent resin then, the dry weight of said polymeric adsorbent is the 8-10 of dried herba fibraureae recisae root or stem weight, is incorporated as the water of 10 times of said aqueous ethanolic solution volumes then; Install on the described macroporous adsorptive resins after stirring 2-3h; Water wash to elutant colourless after, use the organic solvent wash-out again, said volume of organic solvent is a 2-4 times of column volume; Its flow velocity is 0.5-1 times of column volume/h; The elutriant that obtains carries out concentrating under reduced pressure, reclaims organic solvent, obtains being brown buttery herba fibraureae recisae alkaloid extract.Employing HPLC method records the fibranine in this herba fibraureae recisae alkaloid extract, the total content of fibraminine is not less than 33%.
In the present invention, macroporous adsorbent resin is a kind of new non-ionic type organic high molecular polymer sorbent material.The separation and the purification process of Chinese herbal medicine effective ingredients have been widely used in.It is to be monomer with vinylbenzene and propenoate, is linking agent with the divinylbenzene, and toluene, YLENE are pore-creating agent, and their polymerizations that is cross-linked with each other have formed porous skeleton structure.This resin has adsorptivity through Van der Waals force and the hydrogen bond action between itself and the molecule that is adsorbed; Because of its reticulated structure and high-specific surface area have the selectively ability of adsorb organic compound matter, therefore use this resin can realize the purpose of the isolation and purification of herba fibraureae recisae alkaloid extract.
In the present invention, described macroporous adsorbent resin is HPD series macroporous adsorbent resin 100 or 300 models or the close macroporous adsorbent resin of other polarity.This HPD series macroporous adsorbent resin for example is with trade(brand)name HPD series macroporous adsorbent resin product sold by the precious grace chemical industry in Cangzhou ltd.The close macroporous adsorbent resin of other polarity for example is with trade(brand)name HZ series macroporous adsorbent resin product sold by Shanghai Huazhen Science and Technology Co., Ltd..
The granularity of described macroporous adsorbent resin is the 60-16 order, preferably 50-30, more preferably 40-30.
Described macroporous adsorbent resin pre-treatment is to place container with washing 2-3 time from the beginning resin, and the consumption of each water is 1-1.5 a times of resin volume; Again with resin transfer to post, be washed till the ethanol that washes again in the resin 1 part of ethanol does not produce white opacity in three parts of water after with ethanol and get final product.After using repeatedly, polymeric adsorbent darkens, and when adsorption effect descended, available 1mol/L NaOH (or HCl) washing or soak appropriate time was advisable near native color to resin, continues to be washed till neutrality with zero(ppm) water and can to use again.
Described macroporous adsorptive resins is colourless until elutant with big water gaging flushing earlier after absorption; Like this; Can be more fully, up hill and dale water-soluble high polarity impurity such as the carbohydrate of macroporous adsorptive resins absorption, mucus juice are washed away, and then use the polar organic solvent wash-out.
In the present invention, described polar organic solvent is a kind of solvent that is selected from ethanol, methyl alcohol, acetone or ETHYLE ACETATE.In the present invention, described ethanol, methyl alcohol generally are aqueous ethanolic solution, methanol aqueous solution.
Preferably, described polar organic solvent is ethanol or methanol aqueous solution.
The concentration of described polar organic solvent is more than 85% (V/V), and its volume is 2-4 a times of resin column volume.The condition of carrying out wash-out is that elutriant is slowly added in the adsorption column, regulates flow velocity to 0.5-1 times of column volume/h.
(3) the herba fibraureae recisae alkaloid extract that step (2) is obtained uses the dissolving of 90%-98% (V/V) aqueous ethanolic solution with the weight ratio 1 of said extract and said aqueous ethanolic solution: 2-4; Mix with described macroporous adsorbent resin then; The dry weight of described polymeric adsorbent is 8-10 a times of said herba fibraureae recisae alkaloid extract weight, is incorporated as the water of 10 times of said aqueous ethanolic solution volumes then, joins on the described macroporous adsorptive resins behind the stirring 2-3h; Water wash to elutant be colourless after; Earlier use the non-polar organic solvent wash-out, use the polar organic solvent wash-out again, the volume of said polar organic solvent is a 2-4 times of column volume; Its flow velocity is 0.5-1 times of column volume/h, collects the polar organic solvent elutriant;
Macroporous adsorbent resin described in this step is macroporous adsorbent resin 500 or 600 models of HPD series or the macroporous adsorbent resin that other polar phase is worked as.This HPD series macroporous adsorbent resin for example be by by the precious grace chemical industry in Cangzhou ltd with trade(brand)name HPD series macroporous adsorbent resin product sold.The close macroporous adsorbent resin of other polarity for example is with trade(brand)name HZ series macroporous adsorbent resin product sold by Shanghai Huazhen Science and Technology Co., Ltd..
The granularity of described macroporous adsorbent resin is the 60-16 order, preferably 50-30, more preferably 40-30.
Described macroporous adsorbent resin pre-treatment is to place container with washing 2-3 time from the beginning resin, and the consumption of each water is 1-1.5 a times of resin volume; Again with resin transfer to post, be washed till the ethanol that washes again in the resin 1 part of ethanol does not produce white opacity in three parts of water after with ethanol and get final product.After using repeatedly, polymeric adsorbent darkens, and when adsorption effect descended, available 1mol/L NaOH (or HCl) washing or soak appropriate time was advisable near native color to resin, continues to be washed till neutrality with zero(ppm) water and can to use again.
In this step, described non-polar organic solvent is one or more solvents that are selected from sherwood oil, normal hexane, hexanaphthene.
Preferably, described non-polar organic solvent is a sherwood oil.
Described polar organic solvent is a kind of solvent that is selected from ethanol, methyl alcohol, acetone or ETHYLE ACETATE.In the present invention, described ethanol, methyl alcohol generally are aqueous ethanolic solution, methanol aqueous solution.
Preferably, described polar organic solvent is ethanol or methanol aqueous solution.
The concentration of this aqueous ethanolic solution, methanol aqueous solution is more than 95% (V/V).
In the present invention, described effluent volume is 2-4 a times of column volume, and the condition of carrying out wash-out is that elutriant is slowly added in the adsorption column, regulates flow velocity to 0.5-1 times of column volume/h.
(4) the polar organic solvent elutriant that above-mentioned steps (3) is obtained carries out concentrating under reduced pressure; Reclaim organic solvent; The enriched material that obtains is used the recrystallization organic solvent dissolution, at temperature 25-60 ℃ of vibration 15-25min, leaves standstill crystallization then; Recrystallization is carried out in the crystallization that obtains in the recrystallization organic solvent, obtain being the flaky Fibrauretin vegeto-alkali of leaflet crystallized product.
In the present invention, described recrystallization organic solvent is one or more solvents that are selected from sherwood oil, ether or normal hexane, preferably sherwood oil or ether, more preferably sherwood oil.
In the present invention, described concentrating under reduced pressure is under the temperature 30-50 ℃ of condition with vacuum tightness 0.1-0.5MPa, to carry out.
The equipment that said concentrating under reduced pressure uses is with trade(brand)name ZX98-1 Rotary Evaporators product sold by her industry and trade ltd of Shandong, Shanghai.
The flaky Fibrauretin vegeto-alkali of the leaflet crystallized product that is that obtains adopts HPLC method (HPLC) to analyze, and its result shows that this crystallized product contains total 81% above fibranine and fibraminine.
In the present invention, described HPLC assay method is to adjust through suitable in common implementation step of this analytical technology and condition, meets the measuring method that the present invention measures requirement fully.
[beneficial effect]
The present invention preparation to contain in the herba fibraureae recisae alkaloid extract active constituent content higher, the content of fibranine, fibraminine can reach more than 33%.The Fibrauretin crystallization look of producing is snow-white, purity is high, and wherein fibranine, fibraminine total content are more than 81%.
Owing to select macroporous adsorbent resin for use, it is good to the alkaloidal adsorption selectivity of herba fibraureae recisae, and absorption is fast, and desorb is also fast, and loading capacity is bigger; Physical and chemical stability is high, and physical strength is good, and regeneration easily; Operation is very easy, and step is few, and is with low cost, and extraction rate reached is more than 95%, all recyclable utilization of solvent, and environmentally safe is specially adapted to large-scale commercial prodn.
[embodiment]
To illustrate in greater detail the present invention through embodiment below, rather than to the restriction of protection domain of the present invention.
Embodiment 1
Take by weighing Guangdong herba fibraureae recisae root dried powder 200g, 30 ℃ of temperature and constantly stir down with acetone extraction 3 times, 800ml, 1h at every turn at every turn.Filter then, merging filtrate concentrates and reclaims acetone.After the enriched material that obtains dissolved with 30ml 10% ethanol (V/V), the HPD100 mixed with resin with dry weight 1600g added 400ml water again, and constant speed (30rpm) stirs 2h.With the flushing of 1000ml water, flow velocity is 400ml/h, uses 300ml 85% (V/V) alcohol flushing then, flow velocity 75ml/h then.The ethanol eluate that obtains concentrates, and obtains containing herba fibraureae recisae alkaloid extract 1.86g, yield 0.93%, and the HPLC method records fibranine in the extract, the fibraminine total content is 38.25%.
Take by weighing the above-mentioned herba fibraureae recisae alkaloid extract 3.00g that contains, with after 6ml 95% (V/V) the aqueous ethanolic solution dissolving, with dry weight be the HPD600 mixed with resin of 30g, add 100ml water again, stir upper prop behind the 2h.Use the flushing of 500ml water after elutant is colourless, use 300ml sherwood oil wash-out again, flow velocity is 75ml/h.Use 300ml 95% (V/V) ethanol to continue wash-out then, flow velocity is 75ml/h.The concentrating under reduced pressure ethanol eluate reclaims solvent, and the enriched material that obtains is used petroleum ether dissolution, at 50 ℃ of 25min that vibrate down, leaves standstill crystallization then, and the crystallization that obtains is recrystallization once more, obtains snowy white leaflet sheet Fibrauretin crystallization 0.91g.The herba fibraureae recisae vegeto-alkali recovery 82.5%.The HPLC method records and contains fibranine 69.21% in the crystallization, and fibraminine 28.45%, the two total content are 81.66%.
Embodiment 2
Take by weighing the dry powder 200g of herba fibraureae recisae root or stem, at 60 ℃ and constantly stir down with 50% (V/V) extraction using alcohol 2 times, 1200ml, 1h at every turn at every turn.Filter then, merging filtrate concentrates and reclaims ethanol.After the enriched material that obtains dissolved with 40ml 15% ethanol (V/V), the HPD300 mixed with resin with dry weight 2000g added 400ml water again; Constant speed (30rpm) stirs 2h, and with the flushing of 1000ml water, flow velocity is 400ml/h then; Use 270ml 95% (V/V) alcohol flushing again, flow velocity is 120ml/h.The ethanol eluate that obtains concentrates, and obtains containing herba fibraureae recisae alkaloid extract 1.78g, yield 0.89%, and the HPLC method records fibranine in the extract, the fibraminine total content is 38.64%.
Take by weighing the above-mentioned herba fibraureae recisae alkaloid extract 3.00g that contains, with after 6ml 95% (V/V) the aqueous ethanolic solution dissolving, with dry weight be the HPD500 mixed with resin of 25g, add 200ml water again, stir upper prop behind the 3h.Use the flushing of 500ml water after elutant is colourless, use hexanaphthene 250ml wash-out again, flow velocity is 60ml/h.Continue wash-out with 300ml methyl alcohol then, flow velocity is 100ml/h.The concentrating under reduced pressure meoh eluate reclaims solvent, and the enriched material that obtains is used n-hexane dissolution, at 40 ℃ of 25min that vibrate down, leaves standstill crystallization then, and the crystallization that obtains is recrystallization once more, obtains snowy white leaflet sheet Fibrauretin crystallization 0.90g.The herba fibraureae recisae vegeto-alkali recovery 81.3%.The HPLC method records and contains fibranine 69.19% in the crystallization, and fibraminine 28.45%, the two total content are 83.64%.
Embodiment 3
Take by weighing the dry powder 200g of herba fibraureae recisae root or stem, at 60 ℃ and constantly stir down, with 80% extraction using alcohol 3 times, the alcoholic acid amount is 5 times of weight at every turn, at every turn 1h.Filter then, merging filtrate concentrates and reclaims ethanol.Obtain enriched material with after 40ml 20% ethanol (V/V) dissolving, with the HPD300 mixed with resin of dry weight 1800g.Add 400ml water then, constant speed (30rpm) stirs 3h, and with the flushing of 1000ml water, flow velocity is 400ml/h again.Use the 120ml washed with methanol then, flow velocity is 50ml/h.The meoh eluate that obtains concentrates, and obtains containing herba fibraureae recisae alkaloid extract 1.88g, yield 0.94%.The HPLC method records fibranine in the extract, the fibraminine total content is 37.35%.
Take by weighing the above-mentioned herba fibraureae recisae alkaloid extract 3.00g that contains, after the dissolving of 6ml 95% (V/V) aqueous ethanolic solution, the HPD600 mixed with resin with dry weight 25g adds 200ml water again, upper prop behind the stirring 2h.Use the flushing of 500ml water after elutant is colourless, use sherwood oil again: the 300ml mixed solvent wash-out of hexanaphthene=1: 1 (V/V), flow velocity is 75ml/h.Continue wash-out with 300ml acetone then, flow velocity is 75ml/h.Concentrating under reduced pressure acetone elutriant reclaims solvent; The enriched material that obtains is used sherwood oil: the dissolving of ether=1: 1 (V/V) mixed solvent, at 30 ℃ of 25min that vibrate down, leave standstill crystallization then; The crystallization that obtains is recrystallization once more, obtains snowy white leaflet sheet Fibrauretin crystallization 0.92g.The herba fibraureae recisae vegeto-alkali recovery 82.0%.The HPLC method records and contains fibranine 69.21% in the crystallization, and fibraminine 28.52%, the two total content are 85.73%.
Claims (5)
1. method that adopts the macroporous adsorbent resin legal system to be equipped with natural fibrauretine crystal is characterized in that this method steps is following:
(1) get dried herba fibraureae recisae root or stem powder, with an organic solvent the weight ratio 8-10 with said organic solvent and said herba fibraureae recisae root or stem powder at room temperature extracted 1.5-2.5 hour, repeated to extract 2-3 time; United extraction liquid; Carry out concentrating under reduced pressure then, reclaim organic solvent, obtain enriched material;
(2) enriched material that obtains of step (1) uses volume(tric)fraction to dissolve as the aqueous ethanolic solution of 10%-20% with the weight ratio 1 of said enriched material and said aqueous ethanolic solution: 2-4; Mix with macroporous adsorbent resin then, the dry weight of said polymeric adsorbent is dried herba fibraureae recisae root or stem weight 8-10 a times, is incorporated as the water of 10 times of said aqueous ethanolic solution volumes then; Install on the described macroporous adsorptive resins after stirring 2-3h; Water wash to elutant colourless after, use the organic solvent wash-out again, said volume of organic solvent is a 2-4 times of column volume; Its flow velocity is 0.5-1 times of column volume/h; The elutriant that obtains carries out concentrating under reduced pressure, reclaims organic solvent, obtains being brown buttery herba fibraureae recisae alkaloid extract; Macroporous adsorbent resin described in the step (2) is HPD series macroporous adsorbent resin 100 or 300 type macroporous adsorbent resins;
(3) the herba fibraureae recisae alkaloid extract that step (2) is obtained uses the aqueous ethanolic solution dissolving of volume(tric)fraction as 90-98% with the weight ratio 1 of said extract and said aqueous ethanolic solution: 2-4; Mix with described macroporous adsorbent resin then; The dry weight of described polymeric adsorbent is 8-10 a times of said herba fibraureae recisae alkaloid extract weight, is incorporated as the water of 10 times of said aqueous ethanolic solution volumes then, joins on the described macroporous adsorptive resins behind the stirring 2-3h; Water wash to elutant be colourless after; Earlier use the non-polar organic solvent wash-out, use the polar organic solvent wash-out again, the volume of said polar organic solvent is a 2-4 times of column volume; Its flow velocity is 0.5-1 times of column volume/h, collects the polar organic solvent elutriant; The said polar organic solvent that is used for wash-out is ethanol, methyl alcohol, acetone or ETHYLE ACETATE, and wherein said ethanol is volume(tric)fraction greater than 95% aqueous ethanolic solution, and said methyl alcohol and volume(tric)fraction are greater than 95% methanol aqueous solution; Macroporous adsorbent resin described in the step (3) is HPD series macroporous adsorbent resin 500 or 600 type macroporous adsorbent resins;
(4) the polar organic solvent elutriant that step (3) is obtained carries out concentrating under reduced pressure; Reclaim organic solvent; The enriched material that obtains is used the recrystallization organic solvent dissolution, at temperature 25-60 ℃ of vibration 15-25min, leaves standstill crystallization then; Recrystallization is carried out in the crystallization that obtains in the recrystallization organic solvent, obtain being the flaky Fibrauretin vegeto-alkali of leaflet crystallized product.
2. method according to claim 1 is characterized in that be one or more organic solvents that are selected from ethanol, methyl alcohol, acetone or ETHYLE ACETATE in step (1) with the organic solvent described in (2).
3. method according to claim 1 is characterized in that at the non-polar organic solvent described in the step (3) be one or more non-polar organic solvents that are selected from sherwood oil, ether or normal hexane.
4. method according to claim 1 is characterized in that described concentrating under reduced pressure carries out under temperature 30-50 ℃.
5. method according to claim 1 is characterized in that described recrystallization organic solvent is one or more solvents that are selected from sherwood oil, ether or normal hexane.
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| CN106349239A (en) * | 2016-08-25 | 2017-01-25 | 西安天生物技术股份有限公司 | Process method for alcohol extraction of palmatine |
| CN107815348B (en) * | 2017-10-20 | 2021-03-23 | 广州栋方生物科技股份有限公司 | Method for removing safrole from borneol oil |
| CN110437214A (en) * | 2019-09-10 | 2019-11-12 | 杨海鹰 | A kind of purification process of Aloesin |
| CN110975842B (en) * | 2019-12-16 | 2022-09-27 | 健帆生物科技集团股份有限公司 | Immunoadsorbent, preparation method thereof and adsorber for hemoperfusion |
| CN114773358B (en) * | 2022-04-02 | 2024-01-09 | 仲恺农业工程学院 | Method for extracting rotenone from radix Puerariae |
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| 李维莉 等.黄藤素酸提液不同精制方法的比较研究.《昆明学院学报》.2009,第31卷(第3期),48-49. |
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