CN101264128A - Preparation of sophora alopecuroids total alkaloid - Google Patents
Preparation of sophora alopecuroids total alkaloid Download PDFInfo
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- CN101264128A CN101264128A CNA2008100944205A CN200810094420A CN101264128A CN 101264128 A CN101264128 A CN 101264128A CN A2008100944205 A CNA2008100944205 A CN A2008100944205A CN 200810094420 A CN200810094420 A CN 200810094420A CN 101264128 A CN101264128 A CN 101264128A
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Abstract
The invention provides a preparation method of Alkaloids of Sophora alopecuroides, which adopts the process steps such as ultramicro broken-wall shattering, acid-water percolation, flocculater clarifying, hyperfiltration purifying, alkalization extraction, rinse halocarbon layer, decompressing concentration. The invention has the advantages of scientific and rational craft, simple operation, less steps, rapid extraction flow path, high alkalization yield, and overcoming the defects of the prior public technology such as low craft yield, complex craft operation and low applicability. The invention is suitable for industrial large-scale production.
Description
Technical field
The present invention relates to the extraction of Sophora Alopecuroides L. biology total alkali, aim to provide the preparation method of the simple and efficient of Sophora Alopecuroides L. biology total alkali, improve the extraction ratio and the content thereof of Sophora Alopecuroides L. biology total alkali, be applicable to large-scale industrialization production.
Background technology
Sophora Alopecuroides L. (Sophora alopecuroids L) is a cassia leguminous plant, mainly is distributed in temperate zone, subtropical zone, and China concentrates on northwestward desert, half-desert area.Sophora Alopecuroides L. is a herbaceos perennial, and its rhizome and underground bud all can be used as medicine.In China, the area that Sophora Alopecuroides L. distributes is wide, and natural resources is extremely abundant.
Sophora Alopecuroides L. is genuine natural Chinese medicine, includes with matrine, and oxymatrine, sophoridine, Oxysophoridine etc. are western pyridine Alkaloid in the main multiple quino.Through studies have shown that of modern pharmacology, pharmacodynamics aspect, Sophora Alopecuroides L. alkaloid and component thereof have significant antitumor, arrhythmia, anti-inflammation, build up resistance and immunity, resistance state property inflammation and pharmacological actions such as anti-hepatitis B, rising leukocyte.Therefore, various alkaloids all have high medical value in the Sophora Alopecuroides L., and extracting alkaloid from Sophora Alopecuroides L. has high economic benefit and social benefit.
The yield height of total alkaloids when Sophora Alopecuroides L. acid extraction alkaloid extracts, but extracting liquid volume is big, the coexistence of macromolecular substances such as alkaloid and protein, polysaccharide, colloid, ethanol precipitation commonly used removes macromolecular substances, but need consume a large amount of ethanol during ethanol precipitation, and removing macromolecular substances simultaneously, alkaloidal loss is also bigger.(horse Chaoyang such as horse Chaoyang, Wang Hongxin. the alkaloid in the ultrafiltration purification Herba Sophorae alopecuroidis acid extraction thing. Zhengzhou Engineering College's journal 2003,24 (4): 56～58) the alkaloids composition of employing ultrafiltration purification Herba Sophorae alopecuroidis acid extraction thing, it is before adopting ultrafiltration, acid extraction liquid is directly carried out ultrafiltration, and numerous impurity macromole is big to the pressure of filter membrane, and ultrasiltrated rate is slow, need constantly wash film to accelerate ultrasiltrated rate, bring numerous inconvenience to ultra-filtration process.The present invention removes macromole impurity in the acid extraction thing with flocculating agent before ultrafiltration, ultrafiltration can be carried out smoothly.This preparation method has low, the consuming time weak point of production cost, keeps advantages such as composition is many
Summary of the invention
Purpose of the present invention aims to provide the extracting method that a kind of technology is simple, practical, be fit to large-scale industrialization production, Sophora Alopecuroides L. biology total alkali that yield is high.
For achieving the above object, the present invention is by the following technical solutions:
(1) ultra micro wall breaking pulverization: Sophora Alopecuroides L. is handled through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is put into the diafiltration tube, get the sour water percolate with the sour water percolation;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains crude drug amount 0.2-0.8g, add flocculating agent toward concentrated solution in, transferring pH value is between 3～6 to control PH, fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: clear liquid is carried out hyperfiltration treatment by ultrafiltration apparatus, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, gets ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add alkali liquor and transfer PH 〉=10, add low polar organic solvent extraction, behind the standing demix, collected organic layer;
(6) washing halo-hydrocarbon layer: the washing organic layer is neutral until water lotion;
(7) concentrating under reduced pressure: decompression, concentrated organic solvent extraction liquid, drying promptly gets sophora alopecuroids total alkaloid.
The further technical scheme of the present invention is:
(1) ultra micro wall breaking pulverization: Sophora Alopecuroides L. is a 800-1500 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is used the moistening of 5-15% sour water earlier; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 24～48h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out 1～8ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains crude drug amount 0.2-0.8g, adding volume ratio in the concentrated solution is the 2%-4% flocculating agent, and transferring pH value is between 3～6 to control PH, fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 4000-30000 ultrafilter membrane carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 5-15% alkali liquor and transfer PH 〉=10, add low polar organic solvent extraction, behind the standing demix, collected organic layer;
(6) washing halo-hydrocarbon layer: the washing organic layer is neutral until water lotion;
(7) concentrating under reduced pressure: decompression, concentrated organic extract liquid, drying promptly gets sophora alopecuroids total alkaloid.
Among the present invention, it can be organic acid or mineral acid that used adjusting medicinal liquid is tart acid, can be formic acid, acetic acid, fumaric acid, benzoic acid, succinic acid etc. as organic acid, and used mineral acid can be hydrochloric acid, sulphuric acid, nitric acid, carbonic acid etc.Among the present invention, be preferably mineral acid, more preferably hydrochloric acid or sulphuric acid.
Described flocculating agent can be any in chitosan, gelatin, agar, Chinese medicine flocculating agent, 101 fruit juice clarifiers and the ZTC natural clarifying agent, is preferably chitosan.
Among the present invention, the weight percentage in medicinal liquid of flocculating agent can be 0.01%～10%.
Among the present invention, the organic solvent of the medicinal liquid after the extraction alkalization is low polar organic solvent, go into can be halogenated alkane, benzene,toluene,xylene, ether, ethyl acetate etc. some can make the free dissolved low polar organic solvent of alkaloid.In the described halogenated alkane, wherein alkane is meant that carbon atom is the alkane of 1-4, is preferably the alkane of 1-2 carbon atom.Among the present invention, most preferably be the alkane of a carbon atom, as chloroform or dichloromethane.
In the described alkalization extraction process step, add alkali and transfer the alkali of PH to be preferably NaOH or KOH.
Those skilled in the art also can clearly know, used alkali can also be the solution that other can the messenger drug liquid caustic sodaization, as NaHCO
3, Na
2CO
3, KHCO
3, K
2CO
3Deng.
Among the present invention, the used molecular cut off of ultrafilter membrane can be the scope of 4000-30000, and for making the alkaloid purification effect that reaches better, preferred molecular cut off is the film of 6000-10000, more preferably the film of molecular cut off 6000.
The present invention adopts the macromolecular substances in the chitosan absorption sour water percolate, and settled mechanism is: chitosan positively charged (NH
4) with medicinal liquid in the crosslinked and sedimentation of electronegative impurity.This method has low, the consuming time weak point of production cost, keeps advantages such as composition is many.Therefore, compared with prior art, the present invention has following feature and advantage:
(1) technology is reasonable, and is simple to operate, total alkaloid content height in the extract.
(2) technology is practical, is fit to large-scale industrialization production.
(3) non-environmental-pollution.
Do not have generations such as sewage, poison in the whole process of production, used chloroform is recyclable in the production utilizes again, and extraction back Sophora Alopecuroides L. residue can be used as fertilizer and carries out deep layer circulation development and use, not only can increase economic efficiency, and can improve environmental treatment pressure.
Description of drawings
Fig. 1 is that the present invention extracts the process chart that the sophora alopecuroids total alkaloid method is extracted preparation
Specific embodiment
Employed in the present invention term unless other explanation is arranged, generally has the implication of those of ordinary skills' common sense.
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these embodiment just in order to demonstrate the invention, but not limit the scope of the invention by any way.
In following embodiment, various processes of Xiang Ximiaoshuing and method are not conventional methods as known in the art.The source of agents useful for same, trade name and be necessary to list its constituent person indicate when occurring first that all used thereafter identical reagent if no special instructions, and is all identical with the content of indicating first.
Embodiment one
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 800 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 5% hydrochloric acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 24h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 1ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.5g of crude drug amount, the adding volume ratio is 2% flocculating agent in the concentrated solution, and accent pH value to 3 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 6000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 5% alkali liquor accent PH to 10, add the chloroform extraction, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing chloroform layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform extraction liquid, drying promptly gets sophora alopecuroids total alkaloid 63.21%.
Embodiment two
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 1000 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 8% hydrochloric acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 24h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 3ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.6g of crude drug amount, the adding volume ratio is 2% flocculating agent in the concentrated solution, and accent pH value to 4 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 10000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 8% alkali liquor accent PH to 10, add the chloroform extraction, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing halo-hydrocarbon layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform layer extract, drying promptly gets sophora alopecuroids total alkaloid 65.34%.
Embodiment three
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 1200 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 10% hydrochloric acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 36h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 5ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.7g of crude drug amount, the adding volume ratio is 3% flocculating agent in the concentrated solution, and accent pH value to 4.5 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 6000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 10% alkali liquor accent PH to 10, add the chloroform extraction, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing halo-hydrocarbon layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform layer extract, drying promptly gets sophora alopecuroids total alkaloid 67.56%.
Embodiment four
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 1400 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 12% hydrochloric acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 36h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 6ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.7g of crude drug amount, the adding volume ratio is 3% flocculating agent in the concentrated solution, and accent pH value to 5 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 6000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 10% alkali liquor accent PH to 10, add the chloroform extraction, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing halo-hydrocarbon layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform layer extract promptly gets sophora alopecuroids total alkaloid 70.21%.
Embodiment five
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 1500 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 15% hydrochloric acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 36h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 8ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.8g of crude drug amount, the adding volume ratio is 4% flocculating agent in the concentrated solution, and accent pH value to 6 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 6000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 10% alkali liquor accent PH to 10, add the chloroform extraction, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing halo-hydrocarbon layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform layer extract, drying promptly gets sophora alopecuroids total alkaloid 66.14%.
Embodiment six
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 1500 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 5% acetic acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 48h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 5ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.4g of crude drug amount, the adding volume ratio is 4% flocculating agent in the concentrated solution, and accent pH value to 6 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 6000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 10% alkali liquor accent PH to 10, add the chloroform extraction, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing halo-hydrocarbon layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform layer extract, drying promptly gets sophora alopecuroids total alkaloid 62.22%.
Embodiment seven
Concrete extraction process step is as follows:
(1) ultra micro wall breaking pulverization: taking by weighing Sophora Alopecuroides L. 1kg, is 800 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is first with 15% acetic acid water-wet; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 36h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out the 8ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains the about 0.3g of crude drug amount, the adding volume ratio is 3% flocculating agent in the concentrated solution, and accent pH value to 5 fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 6000 ultrafilter membranes carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 8% alkali liquor accent PH to 10, add the chloroform extraction again, behind the standing demix, collect chloroform layer, react to final chloroform layer extract alkaloid and be negative, merge each time chloroform extraction liquid;
(6) washing halo-hydrocarbon layer: the washing chloroform layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure chloroform layer extract, drying promptly gets sophora alopecuroids total alkaloid 60.18%.
Claims (10)
1. the preparation method of Sophora Alopecuroides L. biology total alkali is characterized in that, its step is as follows:
(1) ultra micro wall breaking pulverization: Sophora Alopecuroides L. is handled through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is put into the diafiltration tube, use the sour water percolation, get the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains crude drug amount 0.2-0.8g, add flocculating agent toward concentrated solution in, transferring pH value is between 3～6 to control PH, fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: clear liquid is carried out hyperfiltration treatment by ultrafiltration apparatus, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, gets ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add alkali liquor and transfer PH 〉=10, add low polar organic solvent extraction, behind the standing demix, collected organic layer;
(6) washing halo-hydrocarbon layer: the washing organic layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure organic solvent extraction liquid, drying promptly gets sophora alopecuroids total alkaloid.
2. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 1 is characterized in that, concrete operating procedure is as follows:
(1) ultra micro wall breaking pulverization: Sophora Alopecuroides L. is a 800-1500 purpose ultra micro breaking cellular wall powder through the ultra micro wall breaking pulverization;
(2) sour water diafiltration: the Sophora Alopecuroides L. ultra micro breaking cellular wall powder that step (1) obtains is used the moistening of 5-15% sour water earlier; Try to give a false impression at the end in percolator bottom, and the suitable medical material of place mat, the medicated powder of the moistening compacting layer by layer percolator of packing into, and answer the tense-lax unanimity; Aerofluxus; Dipping is placed 24～48h, makes solvent fully permeate diffusion; Carry out percolation with acid water, every 1kg medical material per minute flows out 1～8ml liquid of filtering, the sour water percolate;
(3) concentrate flocculation: the sour water percolate is condensed into every milliliter contains crude drug amount 0.2-0.8g, adding volume ratio in the concentrated solution is the 2%-4% flocculating agent, and transferring pH value is between 3～6 to control PH, fully stirs, leaves standstill, filtration or centrifugal, gets clear liquid;
(4) ultrafiltration purification: the ultrafiltration apparatus of clear liquid by molecular cut off 4000-30000 ultrafilter membrane carried out hyperfiltration treatment, collect permeate, add sour water in trapped fluid, carry out dilute filtration, filtrate is incorporated permeate into, ultrafiltrate;
(5) alkalization extraction: in ultrafiltrate, add 5-15% alkali liquor and transfer PH 〉=10, add low polar organic solvent extraction, behind the standing demix, collected organic layer;
(6) washing halo-hydrocarbon layer: the washing organic layer is neutral until water lotion;
(7) concentrating under reduced pressure: concentrating under reduced pressure organic solvent extraction liquid, drying promptly gets sophora alopecuroids total alkaloid.
3. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 1 and 2 is characterized in that, the acid in the described sour water is mineral acid or organic acid.
4. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 3 is characterized in that, the acid in the described sour water is preferably hydrochloric acid or sulphuric acid.
5. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 1 and 2, it is characterized in that, described low polar organic solvent can be halogenated alkane, benzene,toluene,xylene, ether, ethyl acetate etc. some can make a kind of in the free dissolved low polar organic solvent of alkaloid.
6. low polar organic solvent according to claim 5 is preferably chloroform or dichloromethane.
7. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 1 and 2, it is characterized in that, described flocculating agent can be any in chitosan, gelatin, agar, Chinese medicine flocculating agent, 101 fruit juice clarifiers and the ZTC natural clarifying agent, and the percentage by weight of flocculating agent and medicinal liquid is 0.01%～10%.
8. according to the preparation method of the described Sophora Alopecuroides L. biology total alkali of stating of claim 6, it is characterized in that described flocculating agent is preferably chitosan.
9. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 1 and 2 is characterized in that, in the described alkalization extraction process step, adds alkali and transfers the alkali of PH to be preferably NaOH or KOH.
10. the preparation method of Sophora Alopecuroides L. biology total alkali according to claim 1 and 2 is characterized in that, ultrafilter membrane is preferably the film that molecular cut off is 6000-10000.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104825533A (en) * | 2015-05-07 | 2015-08-12 | 江苏天晟药业有限公司 | Preparation method of sophora alopecuroides total alkaloid |
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2008
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104825533A (en) * | 2015-05-07 | 2015-08-12 | 江苏天晟药业有限公司 | Preparation method of sophora alopecuroides total alkaloid |
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